CN101177297A - Method for manufacturing high-grade artificial rutile by ilmenite concentrate - Google Patents
Method for manufacturing high-grade artificial rutile by ilmenite concentrate Download PDFInfo
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- CN101177297A CN101177297A CNA200710050327XA CN200710050327A CN101177297A CN 101177297 A CN101177297 A CN 101177297A CN A200710050327X A CNA200710050327X A CN A200710050327XA CN 200710050327 A CN200710050327 A CN 200710050327A CN 101177297 A CN101177297 A CN 101177297A
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Abstract
The invention relates to a preparation method of high-grade synthetic rutile by using ilmenite concentrate. The technological procedure is as followings in sequence: firstly, a ball milling is activated; the mechanical ball milling is implemented to the ilmenite concentrate with a ball mill so as to activate the ilmenite concentrate; secondly, atmospheric pressure leaching; with a ratio ranging from 1:3 to 1:5 in volume, the ilmenite concentrate and the hydrochloric acid solution are heated to 90 to 105 DEG C in atmospheric pressure to carry out the leaching reaction for 4 to 6 hours, thereby a front body of the synthetic rutile is obtained; thirdly, solid-liquid separation, after the reaction is completed, the ground paste is cooled down to 30 DEG C to 50 DEG C, and then the front body of the synthetic rutile is separated from the mother solution by adopting a vacuum filtration, the separated mother solution can be prepared into revival hydrochloric acid and cycled to be used in atmospheric pressure leaching procedures; fourthly, washing, drying and calcining; the front body of the separated synthetic rutile is washed and dried, and then is calcined for 2 to 4 hours at a temperature of 800 DEG C to 1000 DEG C, thereby the powder synthetic rutile is obtained.
Description
Technical field
The invention belongs to the preparation method of artificial rutile, particularly a kind of is the method for feedstock production high-grade artificial rutile with the ilmenite concentrate.
Background technology
The titanium dioxide of the whole world more than 60% adopts the chlorination process explained hereafter at present, its main raw material is a rutile, but natural rutile only accounts for 0.3～1% of titanium resource, so most rutile are to be the artificial rutile that raw material makes with the ilmenite in the chloride process titanium dioxide production.Preparation method about artificial rutile, can be divided into: 1) electrosmelting-lixiviation process, iron in the ilmenite is being reduced into metallic iron more than 1600 ℃, fused iron separates with the slag that contains titanium dioxide (titanium slag), titanium slag obtains artificial rutile through processing steps such as pressurized acid leachings again, such as, U.S. Pat 5830420 and US5063032; 2) preoxidation-reduction-lixiviation process, ferrous iron initial oxidation under temperature more than 800 ℃ restores (for ferrous iron) in the ilmenite, pressurized acid leaching then, such as, U.S. Pat 3967954; 3) reduction-lixiviation process, ferric iron is being reduced to ferrous iron more than 800 ℃ in the ilmenite, pressurized acid leaching then, such as, U.S. Pat 5885324; 4) reduction-rusting process, iron is being reduced into metallic iron more than 1100 ℃ in the ilmenite, corrosion is a hydrous iron oxide in containing small amounts of salts aqueous acid or aqueous ammonium chloride solution then, obtains artificial rutile after separating, calcining, such as Australian Patent 247110.Above-mentioned patent is primarily aimed at the placer type ilmenite resource of weathering and develops, and the purpose of preoxidation is for better reduction, and the reductive purpose is in order to obtain typical ilmenite (FeTiO
3) crystalline structure, improve the leaching performance of mineral.
There is abundant titanium resource in China's Flos Bombacis Malabarici-area, Xichang, and this primary ore iron content 30～34%, vanadium 0.3～1% and titanium 8～14% are referred to as vanadium titano-magnetite, belong to the titanium resource of ore type.This ore deposit obtains calcium-magnesium content (in oxide compound) respectively up to 1～2% and 3～7% ilmenite concentrate after ore dressing.Result of study shows, is raw material with this ilmenite concentrate, no matter is to adopt single smelting process, bubble method or selective chlorination, and calcium magnesium all is difficult to remove, and can only obtain low-grade artificial rutile (TiO
2≤ 80%), such as publication number is the Chinese patent application of CN1128732A.
Publication number is the Chinese invention patent application of CN1552628A, announced that employing weak oxide-hydrochloric acid extract technology handles the method for above-mentioned ore type ilmenite concentrate, its oxidising process is carried out under 680～800 ℃ of temperature, oxygen partial pressure～5% condition, depresses branch and carries out for two sections and leach adding.Publication number is the Chinese invention patent application of CN1923703A, has announced that reduction-corrosion-hydrochloric acid of handling this type of ore deposit leaches route, and its reduction process is being carried out more than 1100 ℃, and the corrosion process reaches 12-18 hour, and the not high (TiO of gained artificial rutile grade
2≤ 88%).
In sum, be that the method for feedstock production artificial rutile has all comprised the high-temperature heat treatment that consumes energy at present with the ilmenite, and wet processing afterwards or use acid pressurization are leached, or employing corrosion processing.The former technology and equipment complexity, latter reaction's overlong time.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, providing a kind of is the method that raw material is made high-grade artificial rutile with the ilmenite concentrate, and this kind method not only technology and equipment is simple, easy to operate, and can cut down the consumption of energy.
The method of manufacturing high-grade artificial rutile of the present invention is a raw material with the ilmenite concentrate, and processing step is as follows successively:
(1) ball milling activation
Adopt ball mill that ilmenite concentrate is carried out mechanical ball milling, make the ilmenite concentrate activation;
(2) normal pressure leaches
The activation ilmenite concentrate is with gram or kilogram metering, and the hydrochloric acid soln of mass concentration 15～25% is with milliliter or rise metering, activation ilmenite concentrate quality: hydrochloric acid soln volume=1: 3～1: 5;
To under normal pressure, be heated to 90～105 ℃ with hydrochloric acid soln by the activation ilmenite concentrate of above-mentioned solid-to-liquid ratio metering and leach reaction, 4～6 hours reaction times, dissolved titanium generation hydrolysis, generation artificial rutile presoma;
(3) solid-liquid separation
After reaction is finished, slip is cooled to 30～50 ℃, adopt the vacuum filtration method that the artificial rutile presoma is separated with mother liquor then, isolated mother liquor makes the muriate of impurity such as iron wherein and the oxide compound that the reaction of oxygen G﹠W generates hydrogenchloride and corresponding impurity through spray roasting, the washings that hydrogenchloride is produced with step (4) absorbs and is prepared into regeneration hydrochloric acid and is circulated to normal pressure and leaches step and use, and realizes the closed cycle of hydrochloric acid;
(4) washing, dry and calcining
Powdered artificial rutile 800～1000 ℃ of calcinings 2～4 hours, is promptly obtained in isolated artificial rutile presoma washing, dry back.
In order to satisfy the requirement of chloride process titanium dioxide production to the rutile granularity, can increase the granulation process step, promptly Powdered artificial rutile is prepared into the artificial rutile of granularity 0.1～1.0mm by tablets press.
In the aforesaid method, ball milling activation balls grinding machine can be selected any in roller ball mill machine, vibromill and the planetary ball mill for use, but the abrading-ball of ball mill and mill tube preferably adopt stainless steel to make.If ball mill is the roller ball grinding machine, preferred activation condition is: the ratio of grinding media to material during ball milling (mass ratio of abrading-ball and ilmenite concentrate) is 40: 1～60: 1, and the mill tube rotating speed is 60～80% of its quick passage critical speed, and the ball milling time is 30～60 minutes.If ball mill is planetary ball mill or vibromill, preferred activation condition is: the ratio of grinding media to material during ball milling (mass ratio of abrading-ball and ilmenite concentrate) is 10: 1～30: 1, and the centrifugal acceleration of abrading-ball is at least 100m/s
2, the ball milling time is 10～20 minutes.
The present invention has following beneficial effect:
1, the method for the invention has improved the reactive behavior of ilmenite by the crystalline structure of ball milling activation destruction ilmenite, therefore can replace traditional high-temperature heat treatment with the ball milling activation, thereby reduce energy consumption significantly.Simultaneously, the leaching performance of activation ilmenite is also improved greatly, can finish under normal pressure and leach reaction, has overcome to leach to be reflected at the technology prejudice of finishing under the pressurized conditions.
2, owing to leach to be reflected under the normal pressure and carry out, thereby reduced requirement, reduced facility investment, simplified technological process leaching plant.
3, the present invention can be suitable in ball milling activation step control ilmenite degree of activation by the resulting preferred activation condition of test, make leach operation obtain loose porous, be easy to filtering solid formation---artificial rutile presoma.
4, solid-liquid separation adopts the vacuum filtration method, can apace solid formation and mother liquor be separated, and has avoided because the solid-liquid separation that efflorescence causes and the difficulty of washing.
5, adopting the artificial rutile of the method for the invention preparation is TiO
2The high-grade artificial rutile of content 〉=91%.
Description of drawings
Fig. 1 is scanning electron microscope (SEM) photo of the artificial rutile presoma that drying step obtained of the method for the invention.
Embodiment
The ball mill that relates among the following embodiment, leaching still, vacuum filtration machine, drying plant, calciner, granulating disc and spray roasting stove etc. are general-purpose equipment, and the commercial goods is arranged.
Embodiment 1
Present embodiment is that raw material is made artificial rutile with Flos Bombacis Malabarici ore type ilmenite concentrate (chemical constitution sees Table 1), and processing step is as follows successively:
(1) ball milling activation
200 gram ilmenite concentrates are carried out the ball milling activation in planetary ball mill, ratio of grinding media to material is 10: 1, and the centrifugal acceleration of abrading-ball is 180m/s
2, the ball milling time is 20 minutes.
(2) normal pressure leaches
The hydrochloric acid soln 500ml that gets 100 gram activatory ilmenites and mass concentration 15% adds the leaching still, under normal pressure, be heated to 90 ℃ and leach reaction, 6 hours reaction times, dissolved titanium generation hydrolysis, generate the artificial rutile presoma, impurity such as dissolved iron are retained in the mother liquor.
(3) solid-liquid separation
After reaction is finished, slip is cooled to 30 ℃, the artificial rutile presoma is separated with mother liquor under the condition of vacuum tightness for-0.06MPa with the vacuum filtration machine then, isolated mother liquor (its composition sees Table 2) is prepared into regeneration hydrochloric acid through spray roasting, hydrogen chloride absorption step and is circulated to normal pressure and leaches step and use;
The operation of spray roasting, hydrogen chloride absorption is as follows:
To leach mother liquor and in the spray roasting stove, under normal pressure, 750 ℃, carry out spray roasting, the hydrogenchloride that roasting generates absorbs with the aqueous hydrochloric acid (this aqueous hydrochloric acid is a washing filter cakes water in the step (4)) of mass concentration about 3%, and the acquisition mass concentration is about 18% hydrochloric acid soln.The rate of recovery of chlorine is 97% in the mother liquor.
(4) washing, dry and calcining
Respectively mass concentration 2% hydrochloric acid soln and each 100ml of tap water are joined in the vacuum filter the filter cake after the solid-liquid separation in vacuum (vacuum tightness-0.06MPa) wash under the condition, then with filter cake in baking oven in normal pressure, 100 ℃ dry 4 hours down, dried artificial rutile presoma (its form is seen Fig. 1) is put into retort furnace and is warming up to 800 ℃ of calcinings 4 hours, promptly obtain Powdered artificial rutile, about its median size 1 μ m, its chemical constitution sees Table 1, as can be seen from Table 1, the content of titanium dioxide is 91.9%.
The chemical constitution of table 1 Flos Bombacis Malabarici ilmenite concentrate and artificial rutile (wt.%)
| TiO 2 | FeO | Fe 2O 3 | SiO 2 | MgO | CaO | Al 2O 3 | MnO 2 | |
| Raw ore | 47.25 | 34.21 | 5.56 | 2.75 | 6.23 | 1.08 | 1.49 | 0.61 |
| Artificial rutile | 91.9 | 2.4 | 5.1 | 0.13 | 0.2 | 0.07 | 0.03 |
Table 2 leaches mother liquor and forms
| Composition | HCl | FeCl 2 | FeCl 3 | MgCl 2 | CaCl 2 | AlCl 3 | MnCl 2 |
| Mass concentration, % | 3.5％ | 9.4％ | 2.5％ | 3.1％ | 0.24％ | 0.45％ | 0.22％ |
Embodiment 2
Present embodiment is that raw material is made artificial rutile with Flos Bombacis Malabarici ore type ilmenite concentrate (chemical constitution sees Table 1), and processing step is as follows successively:
(1) ball milling activation
200 gram ilmenite concentrates are carried out the ball milling activation in planetary ball mill, ratio of grinding media to material is 20: 1, and the centrifugal acceleration of abrading-ball is 100m/s
2, the ball milling time is 15 minutes.
(2) normal pressure leaches
The hydrochloric acid soln 400ml that gets 100 gram activatory ilmenites and mass concentration 20% adds the leaching still, under normal pressure, be heated to 100 ℃ and leach reaction, 6 hours reaction times, dissolved titanium generation hydrolysis, generate the artificial rutile presoma, impurity such as dissolved iron are retained in the mother liquor.
(3) solid-liquid separation
After reaction is finished, slip is cooled to 40 ℃, the artificial rutile presoma is separated with mother liquor under the condition of vacuum tightness for-0.06MPa with the vacuum filtration machine then, isolated mother liquor is prepared into regeneration hydrochloric acid through spray roasting, hydrogen chloride absorption step and is circulated to normal pressure and leaches step and use;
The operation of spray roasting, hydrogen chloride absorption is identical with embodiment 1.
(4) washing, dry and calcining
Washing operation is identical with embodiment 1, after the washing with filter cake in baking oven in normal pressure, 100 ℃ dry 2 hours down, dried artificial rutile presoma is put into retort furnace and is warming up to 1000 ℃ of calcinings 2 hours, promptly obtain Powdered artificial rutile, about its median size 1 μ m, its chemical constitution sees Table 3, and as can be seen from Table 3, the content of titanium dioxide is 92.3%.
The chemical constitution (wt.%) of table 3 gained artificial rutile product
| TiO 2 | Fe 2O 3 | SiO 2 | MgO | CaO | Al 2O 3 | MnO 2 | |
| Product | 92.3 | 2.1 | 5.21 | 0.1 | 0.18 | 0.064 | 0.026 |
Embodiment 3
Present embodiment is that raw material is made artificial rutile with Flos Bombacis Malabarici ore type ilmenite concentrate (chemical constitution sees Table 1), and processing step is as follows successively:
(1) ball milling activation
200 gram ilmenite concentrates are carried out the ball milling activation in planetary ball mill, ratio of grinding media to material is 30: 1, and the centrifugal acceleration of abrading-ball is 100m/s
2, the ball milling time is 10 minutes.
(2) normal pressure leaches
The hydrochloric acid soln 300ml that gets 100 gram activatory ilmenites and mass concentration 25% adds the leaching still, under normal pressure, be heated to 105 ℃ and leach reaction, 4 hours reaction times, dissolved titanium generation hydrolysis, generate the artificial rutile presoma, impurity such as dissolved iron are retained in the mother liquor.
(3) solid-liquid separation
After reaction is finished, slip is cooled to 40 ℃, the artificial rutile presoma is separated with mother liquor under the condition of vacuum tightness-0.06MPa with the vacuum filtration machine then, isolated mother liquor is prepared into regeneration hydrochloric acid through spray roasting, hydrogen chloride absorption step and is circulated to the use of normal pressure leaching step;
The operation of spray roasting, hydrogen chloride absorption is identical with embodiment 1.
(4) washing, dry and calcining
Washing operation is identical with embodiment 1, after the washing with filter cake in baking oven in normal pressure, 200 ℃ dry 1 hour down, dried artificial rutile presoma is put into retort furnace and is warming up to 1000 ℃ of calcinings 2 hours, promptly obtain Powdered artificial rutile, about its median size 1 μ m, its chemical constitution sees Table 4, and as can be seen from Table 4, the content of titanium dioxide is 92.2%.
The chemical constitution (wt.%) of table 4 gained artificial rutile product
| TiO 2 | Fe 2O 3 | SiO 2 | MgO | CaO | Al 2O 3 | MnO 2 | |
| Product | 92.2 | 2.2 | 5.2 | 0.11 | 0.19 | 0.06 | 0.02 |
Embodiment 4
Present embodiment is that raw material is made artificial rutile with Flos Bombacis Malabarici ore type ilmenite concentrate (chemical constitution sees Table 1), and processing step is as follows successively:
(1) ball milling activation
150 gram ilmenite concentrates are carried out ball milling activation in vibromill, be 310m/s based on the centrifugal acceleration of the abrading-ball of vibrational frequency and magnitude determinations
2, ratio of grinding media to material is 10: 1, the ball milling time is 10 minutes.
(2) normal pressure leaches
The hydrochloric acid soln 300ml that gets 100 gram activatory ilmenites and mass concentration 25% adds the leaching still, under normal pressure, be heated to 90 ℃ and leach reaction, 6 hours reaction times, dissolved titanium generation hydrolysis, generate the artificial rutile presoma, impurity such as dissolved iron are retained in the mother liquor.
(3) solid-liquid separation
After reaction is finished, slip is cooled to 50 ℃, the artificial rutile presoma is separated with mother liquor under the condition of vacuum tightness-0.06MPa with the vacuum filtration machine then, isolated mother liquor is prepared into regeneration hydrochloric acid through spray roasting, hydrogen chloride absorption step and is circulated to the use of normal pressure leaching step;
The operation of spray roasting, hydrogen chloride absorption is identical with embodiment 1.
(4) washing, dry and calcining
Washing operation is identical with embodiment 1, after the washing with filter cake in baking oven in normal pressure, 100 ℃ dry 3 hours down, dried artificial rutile presoma is put into retort furnace and is warming up to 800 ℃ of calcinings 4 hours, promptly obtain Powdered artificial rutile, about its median size 1 μ m, its chemical constitution sees Table 5, and as can be seen from Table 5, the content of titanium dioxide is 92.4%.
The chemical constitution (wt.%) of table 5 gained artificial rutile product
| TiO 2 | Fe 2O 3 | SiO 2 | MgO | CaO | Al 2O 3 | MnO 2 | |
| Product | 92.4 | 2.0 | 5.3 | 0.11 | 0.16 | 0.05 | 0.02 |
Embodiment 5
Present embodiment is that raw material is made artificial rutile with Flos Bombacis Malabarici ore type ilmenite concentrate (chemical constitution sees Table 1), and processing step is as follows successively:
(1) ball milling activation
150 gram ilmenite concentrates are carried out ball milling activation in vibromill, be 100m/s based on the centrifugal acceleration of the abrading-ball of vibrational frequency and magnitude determinations
2, ratio of grinding media to material is 30: 1, the ball milling time is 20 minutes.
(2) normal pressure leaches
The hydrochloric acid soln 500ml that gets 100 gram activatory ilmenites and mass concentration 15% adds the leaching still, under normal pressure, be heated to 105 ℃ and leach reaction, 4 hours reaction times, dissolved titanium generation hydrolysis, generate the artificial rutile presoma, impurity such as dissolved iron are retained in the mother liquor.
(3) solid-liquid separation
After reaction is finished, slip is cooled to 40 ℃, the artificial rutile presoma is separated with mother liquor under the condition of vacuum tightness-0.06MPa with the vacuum filtration machine then, isolated mother liquor is prepared into regeneration hydrochloric acid through spray roasting, hydrogen chloride absorption step and is circulated to the use of normal pressure leaching step;
The operation of spray roasting, hydrogen chloride absorption is identical with embodiment 1.
(4) washing, dry and calcining
Washing operation is identical with embodiment 1, after the washing with filter cake in baking oven in normal pressure, 200 ℃ dry 1 hour down, dried artificial rutile presoma is put into retort furnace and is warming up to 1000 ℃ of calcinings 2 hours, promptly obtain Powdered artificial rutile, about its median size 1 μ m, its chemical constitution sees Table 6, and as can be seen from Table 6, the content of titanium dioxide is 92.0%.
The chemical constitution (wt.%) of table 6 gained artificial rutile product
| TiO 2 | Fe 2O 3 | SiO 2 | MgO | CaO | Al 2O 3 | MnO 2 | |
| Product | 92.0 | 2.3 | 5.2 | 0.13 | 0.2 | 0.07 | 0.03 |
Embodiment 6
Present embodiment is that raw material is made artificial rutile with Flos Bombacis Malabarici ore type ilmenite concentrate (chemical constitution sees Table 1), and processing step is as follows successively:
(1) ball milling activation
1000 gram ilmenite concentrates are carried out the ball milling activation in the roller ball grinding machine, ratio of grinding media to material is 40: 1, and the mill tube rotating speed is 240r/min (critical velocity is 300r/min), and the ball milling time is 30 minutes.
(2) normal pressure leaches
The hydrochloric acid soln 300ml that gets 100 gram activatory ilmenites and mass concentration 25% adds the leaching still, under normal pressure, be heated to 90 ℃ and leach reaction, 6 hours reaction times, dissolved titanium generation hydrolysis, generate the artificial rutile presoma, impurity such as dissolved iron are retained in the mother liquor.
(3) solid-liquid separation
After reaction is finished, slip is cooled to 30 ℃, the artificial rutile presoma is separated with mother liquor under the condition of vacuum tightness-0.06MPa with the vacuum filtration machine then, isolated mother liquor is prepared into regeneration hydrochloric acid through spray roasting, hydrogen chloride absorption step and is circulated to the use of normal pressure leaching step;
The operation of spray roasting, hydrogen chloride absorption is identical with embodiment 1.
(4) washing, dry and calcining
Washing operation is identical with embodiment 1, after the washing with filter cake in baking oven in normal pressure, 100 ℃ dry 3 hours down, dried artificial rutile presoma is put into retort furnace and is warming up to 800 ℃ of calcinings 3 hours, promptly obtain Powdered artificial rutile, about its median size 1 μ m, its chemical constitution sees Table 7, and as can be seen from Table 7, the content of titanium dioxide is 91.2%.
The chemical constitution (wt.%) of table 7 gained artificial rutile product
| TiO 2 | Fe 2O 3 | SiO 2 | MgO | CaO | Al 2O 3 | MnO 2 | |
| Product | 91.2 | 3.4 | 5.0 | 0.15 | 0.22 | 0.08 | 0.03 |
Embodiment 7
Present embodiment is that raw material is made artificial rutile with Flos Bombacis Malabarici ore type ilmenite concentrate (chemical constitution sees Table 1), and processing step is as follows successively:
(1) ball milling activation
1000 gram ilmenite concentrates are carried out the ball milling activation in the roller ball grinding machine, ratio of grinding media to material is 60: 1, and grinding simple rotating speed is 180r/min (critical velocity is 300r/min), and the ball milling time is 60 minutes.
(2) normal pressure leaches
The hydrochloric acid soln 500ml that gets 100 gram activatory ilmenites and mass concentration 15% adds the leaching still, under normal pressure, be heated to 105 ℃ and leach reaction, 4 hours reaction times, dissolved titanium generation hydrolysis, generate the artificial rutile presoma, impurity such as dissolved iron are retained in the mother liquor.
(3) solid-liquid separation
After reaction is finished, slip is cooled to 50 ℃, the artificial rutile presoma is separated with mother liquor under the condition of vacuum tightness-0.06MPa with the vacuum filtration machine then, isolated mother liquor is prepared into regeneration hydrochloric acid through spray roasting, hydrogen chloride absorption step and is circulated to the use of normal pressure leaching step;
The operation of spray roasting, hydrogen chloride absorption is identical with embodiment 1.
(4) washing, dry and calcining
Washing operation is identical with embodiment 1, after the washing with filter cake in baking oven in normal pressure, 200 ℃ dry 1 hour down, dried artificial rutile presoma is put into retort furnace and is warming up to 1000 ℃ of calcinings 2.5 hours, promptly obtain Powdered artificial rutile, about its median size 1 μ m, its chemical constitution sees Table 8, and as can be seen from Table 8, the content of titanium dioxide is 91.5%.
The chemical constitution (wt.%) of table 8 gained artificial rutile product
| TiO 2 | Fe 2O 3 | SiO 2 | MgO | CaO | Al 2O 3 | MnO 2 | |
| Product | 91.5 | 3.0 | 5.0 | 0.14 | 0.21 | 0.07 | 0.03 |
Embodiment 8
With the Powdered artificial rutile of the foregoing description gained in granulating disc; polyvinyl alcohol water solution with mass concentration 0.5～1.0% carries out granulation as binding agent; polyvinyl alcohol water solution volume (milliliter): Powdered artificial rutile quality (gram)=1: 10～15; product after the granulation in baking oven in normal pressure, 200 ℃ of dryings 1～2 hour; obtaining granularity is the artificial rutile of 0.2～0.4mm, and this product granularity meets the requirement (0.1～1.0mm) of chloride process titanium dioxide fluidizing chlorination to granularity.
Claims (5)
1. make the method for high-grade artificial rutile with ilmenite concentrate for one kind, it is characterized in that processing step is as follows successively:
(1) ball milling activation
Adopt ball mill that ilmenite concentrate is carried out mechanical ball milling, make the ilmenite concentrate activation;
(2) normal pressure leaches
The activation ilmenite concentrate is with gram or kilogram metering, and the hydrochloric acid soln of mass concentration 15～25% is with milliliter or rise metering, activation ilmenite concentrate quality: hydrochloric acid soln volume=1: 3～1: 5;
To under normal pressure, be heated to 90～105 ℃ by the activation ilmenite concentrate of above-mentioned solid-to-liquid ratio metering and hydrochloric acid soln and leach reaction, in 4～6 hours reaction times, obtain the artificial rutile presoma;
(3) solid-liquid separation
After reaction is finished, slip is cooled to 30～50 ℃, adopts the vacuum filtration method that the artificial rutile presoma is separated with mother liquor then, isolated mother liquor is prepared into regeneration hydrochloric acid through spray roasting, hydrogen chloride absorption step and is circulated to the use of normal pressure leaching step;
(4) washing, dry and calcining
Powdered artificial rutile 800～1000 ℃ of calcinings 2～4 hours, is promptly obtained in isolated artificial rutile presoma washing, dry back.
2. the method with ilmenite concentrate manufacturing high-grade artificial rutile according to claim 1 is characterized in that processing step also comprises granulation, promptly by tablets press Powdered artificial rutile is prepared into the artificial rutile that granularity is 0.1～1.0mm.
3. the method with ilmenite concentrate manufacturing high-grade artificial rutile according to claim 1 and 2 is characterized in that the abrading-ball of ball milling activation step balls grinding machine and mill tube adopt stainless steel to make.
4. the method for making high-grade artificial rutile with ilmenite concentrate according to claim 3, it is characterized in that ball milling activation step balls grinding machine is the roller ball grinding machine, ratio of grinding media to material during ball milling is 40: 1～60: 1, the mill tube rotating speed is 60～80% of its quick passage critical speed, and the ball milling time is 30～60 minutes.
5. the method for making high-grade artificial rutile with ilmenite concentrate according to claim 3, it is characterized in that ball milling activation step balls grinding machine is planetary ball mill or vibromill, ratio of grinding media to material during ball milling is 10: 1～30: 1, and the centrifugal acceleration of abrading-ball is at least 100m/s
2, the ball milling time is 10～20 minutes.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2011026434A1 (en) * | 2009-09-02 | 2011-03-10 | 沙立林 | Titaniumrich hydrochloric acid leaching residue,use thereof and preparation method of titanium dioxide |
| CN102352437A (en) * | 2011-09-15 | 2012-02-15 | 沙立林 | Method for treating hydrochloric acid leachate of ferrotitanium materials |
| CN101746817B (en) * | 2008-12-05 | 2012-06-06 | 攀钢集团钢铁钒钛股份有限公司 | Purification device and method of purifying modified ilmenite concentrate with purification device |
| CN107460331A (en) * | 2016-06-02 | 2017-12-12 | 昆明冶金高等专科学校 | A kind of method that titanium slag is modified |
| CN113716604A (en) * | 2021-08-09 | 2021-11-30 | 武汉工程大学 | Artificial rutile and preparation method thereof |
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2007
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| CN101746817B (en) * | 2008-12-05 | 2012-06-06 | 攀钢集团钢铁钒钛股份有限公司 | Purification device and method of purifying modified ilmenite concentrate with purification device |
| WO2011026434A1 (en) * | 2009-09-02 | 2011-03-10 | 沙立林 | Titaniumrich hydrochloric acid leaching residue,use thereof and preparation method of titanium dioxide |
| RU2518860C2 (en) * | 2009-09-02 | 2014-06-10 | ША Лилинь | Titanium-enriched ilmenite residue, its application and method of obtaining titanium pigment |
| US9206055B2 (en) | 2009-09-02 | 2015-12-08 | Lilin Sha | Titaniumrich hydrochloric acid leaching residue, use thereof and preparation method of titanium dioxide |
| CN102352437A (en) * | 2011-09-15 | 2012-02-15 | 沙立林 | Method for treating hydrochloric acid leachate of ferrotitanium materials |
| CN102352437B (en) * | 2011-09-15 | 2013-06-19 | 沙立林 | Method for treating hydrochloric acid leachate of ferrotitanium materials |
| CN107460331A (en) * | 2016-06-02 | 2017-12-12 | 昆明冶金高等专科学校 | A kind of method that titanium slag is modified |
| CN113716604A (en) * | 2021-08-09 | 2021-11-30 | 武汉工程大学 | Artificial rutile and preparation method thereof |
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