CN108910942A - A method of synthetic rutile is prepared by high calcium magnesium titanium slag - Google Patents
A method of synthetic rutile is prepared by high calcium magnesium titanium slag Download PDFInfo
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- CN108910942A CN108910942A CN201811172625.0A CN201811172625A CN108910942A CN 108910942 A CN108910942 A CN 108910942A CN 201811172625 A CN201811172625 A CN 201811172625A CN 108910942 A CN108910942 A CN 108910942A
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The present invention relates to a kind of method for preparing synthetic rutile by high calcium magnesium titanium slag, this method include oxidizing roasting, reduction sodium roasting, acidleach removal of impurities, calcining and etc. etc. four steps.It is high for the titanium slag calcium-magnesium content of ilmenite production, it is not suitable as the raw material problem of fluidizing chlorination, the impurity content in titanium slag, especially calcium and magnesium can be effectively reduced using the method in the present invention.The synthetic rutile that purity is 91.45% has been prepared by means of the present invention, and impurity removal effect is preferable, and calcium and magnesium total content is below 2%.The raw material used in the present invention is the acid-dissolved titanium slag as made from the ilmenite of Panxi Area, Sichuan Province.
Description
Technical field
The present invention relates to a kind of methods for preparing synthetic rutile by high calcium magnesium titanium slag, belong to chemical industry metallurgical field.
Background technique
The ilmenite in China is resourceful, and Panxi Area, Sichuan Province possesses the titanium ore in China 90%, but the ilmenite knot of this area
Structure is fine and close, and obtained ilmenite concentrate titanium grade is low, and calcium-magnesium content is high, mainly as the raw material of sulfate process titanium dioxide.It gradually sends out in recent years
The chloride process titanium dioxide technique that exhibition is got up is more environmentally friendly compared with sulfuric acid process, efficiently, obtained titanium white chloride product reducing power greatly, impurity
Less, uniform particle sizes, good dispersion.But requirement of the titanium white chloride to raw material is relatively high, production is main or former by import
Material.
In order to make full use of the titanium ore resource in China, the high contents of calcium and magnesium titanium that many enterprises and scientific research institution begin one's study with China
Iron ore prepares the synthetic rutile for being suitble to fluidizing chlorination.It mostly uses greatly at present and ilmenite progress electro-smelting is obtained into titanium slag, then
Titanium slag is prepared into the higher synthetic rutile product of titanium grade by a series of modifications.
CN102745743A Chinese patent literature discloses a kind of method for preparing synthetic rutile with titanium slag, this method
It is that titanium slag is first subjected to high temperature oxidation roasting, obtains modified titanium slag using reduction roasting.The Modified Titanium hydrochloric acid for dreg that will be obtained
One section of normal pressure and multistage counter current fluidization acidleach removal of impurities are carried out, synthetic rutile product can be obtained after drying and calcining.This method
The calcium-magnesium content for the raw material titanium slag used is relatively low, can obtain the relatively high rutile product of titanium grade, but be not suitable for calcium and magnesium
High calcium magnesium titanium slag made from the higher titanium slag of content, the especially ilmenite in Sichuan area.
CN107399758A Chinese patent literature discloses a kind of method for preparing synthetic rutile by high titanium slag, the party
Method is by crushing high titanium slag, alkali leaching is miscellaneous, modified roasting, acidleach slagging-off, calcining, prepares and is able to satisfy chlorination
The rutile raw material that method requires.Method in the patent for the titanium slag that titanium grade is higher, impurity content is few upgrading effect compared with
It is good, for high calcium magnesium titanium slag, it is bad to upgrade effect.And roasting will lead to due to the addition of sodium carbonate in modified firing stage
There is sintering phenomenon in product.
CN104860347A Chinese patent literature also discloses a kind of people in the preparation method of rutile, and this method includes
Acid-dissolved titanium slag modification, acid removal of impurities and calcining step, have obtained the artificial golden red of suitable chloridising manufacturing technique requirent
Stone, purity is up to 91% or more.Microwave reactor used in this method is not suitable for large-scale production, and this method contains suitable for calcium and magnesium
Low titanium slag is measured, the high calcium magnesium titanium slag of Panzhihua Region is unsuitable for.
And acid sludge is required to the artificial gold tested after fine grinding, produced in this way in patent disclosed in major part
The granularity of red stone product is meticulous, needs by further processing（Such as：It is granulated）It could become and meet chloridising production requirement
Raw material increases burden for the processing of subsequent raw material.The advantage and disadvantage for analyzing the prior art form this specially by continuously improving
The method of benefit, this patent are modified experiment to 20 ~ 160 mesh bulky grain titanium slags, and available granularity and impurity content meet
The rutile product that chloridising requires.
Summary of the invention
The object of the invention, which is that, overcomes above-mentioned deficiency, provides a kind of side that synthetic rutile is prepared by high calcium magnesium titanium slag
Method, to achieve the purpose that on the one hand reaching high calcium magnesium titanium slag recycles, and on the other hand reaches the rutile of preparation high-quality
Purpose.Used technical solution is the present invention to solve above-mentioned technical problem：
To achieve the above object, the present invention is to be achieved through the following technical solutions：
A method of synthetic rutile is prepared by high calcium magnesium titanium slag, is included the following steps：
The first step, oxidizing roasting carry out 1 ~ 2h oxidizing roasting, obtain by high calcium magnesium titanium slag under the conditions of 900 DEG C ~ 1050 DEG C of temperature
To oxidation titanium slag；
Second step, restore sodium roasting, the oxidation titanium slag and sodium carbonate that the first step is obtained after mixing, 850 DEG C ~ 1000
1 ~ 2h is carried out at DEG C and restores sodium roasting, obtains modified sodium titanium slag；
Third step, acidleach removal of impurities uniformly mix the sodium titanium slag that second step obtains with the inorganic acid that concentration is 15 ~ 25wt%, and
Fluidized state is heated the mixture in 10-30 minutes and then carries out back flow reaction, is then existed to the residue after back flow reaction
Acidleach in 3-5 hours is carried out in inorganic acid, and finally the residue under acidleach state is filtered, washed and dried, obtains acid
The miscellaneous slag of leaching；
4th step, calcining, the acidleach removal of impurities slag that third step is obtained moves into crucible, under the conditions of 850 DEG C ~ 1000 DEG C of temperature
The calcining for carrying out 1 ~ 2h obtains the synthetic rutile.
Further, in the first step, high calcium magnesium titanium slag is not finely ground electro-titanium slag, is chosen between 20 ~ 160 mesh
Particle, wherein+20 mesh particle fraction≤1%, average particle size is 250 ~ 500 μm.
Further, high calcium magnesium titanium slag is made of following parts by weight substance in the first step： FeO7~13wt%,CaO 1~
3 ~ 6wt% of 2wt%, MgO, surplus TiO2.
Further, in second step, titanium slag is aoxidized before mixing with sodium carbonate, is crushed first, make to aoxidize titanium slag most
Major diameter is not more than 1 millimeter.
Further, when being roasted and being calcined, oxygen content is not less than 21% in burner hearth for the first step and the 4th step,
It is one of coal, coal gas, hydrogen, petroleum coke or two kinds any that second step, which carries out the reducing agent selected when reduction sodium roasting,
It is mixed with arbitrary proportion.
Further, in second step, when oxidation titanium slag is mixed with sodium carbonate, sodium carbonate usage amount is oxidation titanium slag usage amount
20-40%.
Further, inorganic acid is any one in technical hydrochloric acid or sulfuric acid in third step.
Further, the mixed proportion in third step between sodium titanium slag and inorganic acid is：1：8—12.
Further, when third step drying operation, drying temperature is 100-120 DEG C, and drying time is 1-2 hours, is done
Dry post-job water content is not more than 3%.
Compared with the prior art, the invention has the beneficial effects that：
High calcium magnesium titanium slag-oxidizing roasting of the invention-reduction sodium roasting-acidleach removal of impurities-calcining technique, can effectively mention
The removal rate of high impurity promotes the titanium grade of synthetic rutile.The preparation method of synthetic rutile of the present invention can be extensive
Suitable for the electro-titanium slag of the impurity elements such as calcium and magnesium can not be effectively removed by general traditional handicraft, it is particularly suitable for Panzhihua
The high calcium magnesium titanium slag of regional ilmenite production.In the process of the invention, further fine grinding is not needed after titanium slag used is broken, is saved
Labour is saved, equipment is reduced and uses.In the process of the invention, oxidizing roasting makes a part of anosovite be changed into rutile knot
Structure, and then make the more thorough of anosovite structure destruction in the reduction sodium roasting stage.And reduction phase Fe3+ fundamental transformation
For Fe2+, it is more advantageous to next step acidleach removal of impurities.In the process of the invention, acid leaching stage can be replaced with industrial waste acid,
Realize waste utilization.Rutile preparation method of the invention can be used to handle high calcium magnesium titanium slag, the low, calcium-magnesium content by titanium grade
High electro-titanium slag makes full use of, and obtains the raw material-synthetic rutile for being able to satisfy fluidizing chlorination requirement.
Detailed description of the invention
Fig. 1 is the method for the present invention flow chart；
Fig. 2 is the X-ray diffractogram of titanium slag and synthetic rutile in the embodiment of the present invention；
Wherein：A be untreated high calcium magnesium titanium slag 1.；The X-ray diffractogram of the synthetic rutile of b preparation 1.；C is without place
The high calcium magnesium titanium slag of reason is 2.；D is the X-ray diffractogram of the synthetic rutile of preparation 2.；E is untreated high calcium magnesium titanium slag
③；F is the X-ray diffractogram of the synthetic rutile of preparation 3..
Specific embodiment
Embodiment 1
As illustrated in fig. 1 and 2, a method of synthetic rutile is prepared by high calcium magnesium titanium slag, is included the following steps：
The first step, oxidizing roasting carry out 2h oxidizing roasting, obtain titanium oxide by high calcium magnesium titanium slag under the conditions of 900 DEG C of temperature
Slag；
Second step, restore sodium roasting, the oxidation titanium slag and sodium carbonate that the first step is obtained after mixing, at 850 DEG C into
Row 2h restores sodium roasting, obtains modified sodium titanium slag；
Third step, acidleach removal of impurities uniformly mix the sodium titanium slag that second step obtains with the inorganic acid that concentration is 1wt%, and 10
Fluidized state is heated the mixture in minute and then carries out back flow reaction, then in mineral acid to the residue after back flow reaction
Acidleach in 3 hours is carried out, finally the residue under acidleach state is filtered, washed and dried, obtains acidleach removal of impurities slag；
4th step, calcining, the acidleach removal of impurities slag that third step is obtained move into crucible, carry out 2h's under the conditions of 850 DEG C of temperature
Calcining obtains the synthetic rutile.
In the present embodiment, in the first step, high calcium magnesium titanium slag is not finely ground electro-titanium slag, chooses between 20 mesh
Grain, wherein+20 mesh particle fraction≤1%, average particle size is 250 μm.
In the present embodiment, high calcium magnesium titanium slag is made of following parts by weight substance in the first step： FeO7wt%,CaO
1wt%, MgO 3wt%, surplus TiO2.
In the present embodiment, in second step, titanium slag is aoxidized before mixing with sodium carbonate, is crushed first, make to aoxidize titanium slag
Maximum gauge is not more than 1 millimeter.
In the present embodiment, when being roasted and being calcined, oxygen content is 21%, second in burner hearth for the first step and the 4th step
It is coal that step, which carries out the reducing agent selected when reduction sodium roasting,.
In the present embodiment, in second step, when oxidation titanium slag is mixed with sodium carbonate, sodium carbonate usage amount is that oxidation titanium slag uses
The 20% of amount.
In the present embodiment, inorganic acid is technical hydrochloric acid in third step.
In the present embodiment, the mixed proportion in third step between sodium titanium slag and inorganic acid is：1：8.
In the present embodiment, when third step drying operation, drying temperature is 100 DEG C, and drying time is 2 hours, drying operation
Water content afterwards is not more than 3%.
Embodiment 2
As illustrated in fig. 1 and 2, a method of synthetic rutile is prepared by high calcium magnesium titanium slag, is included the following steps：
The first step, oxidizing roasting carry out 1h oxidizing roasting, obtain titanium oxide by high calcium magnesium titanium slag under the conditions of 1050 DEG C of temperature
Slag；
Second step, restore sodium roasting, the oxidation titanium slag and sodium carbonate that the first step is obtained after mixing, at 1000 DEG C into
Row 1h restores sodium roasting, obtains modified sodium titanium slag；
Third step, acidleach removal of impurities uniformly mix the sodium titanium slag that second step obtains with the inorganic acid that concentration is 25wt%, and
Fluidized state is heated the mixture in 30 minutes and then carries out back flow reaction, then to the residue after back flow reaction in inorganic acid
Middle progress acidleach in 5 hours is finally filtered, washed and is dried to the residue under acidleach state, and acidleach removal of impurities slag is obtained；
4th step, calcining, the acidleach removal of impurities slag that third step is obtained move into crucible, carry out 2h under the conditions of 1000 DEG C of temperature
Calcining, obtain the synthetic rutile.
In the present embodiment, in the first step, high calcium magnesium titanium slag is not finely ground electro-titanium slag, is chosen between 160 mesh
Particle, wherein+20 mesh particle fraction≤1%, average particle size is 500 μm.
High calcium magnesium titanium slag is made of following parts by weight substance in the first step in the present embodiment： FeO13wt%,CaO wt%,
MgO 6wt%, surplus TiO2.
In the present embodiment, in second step, titanium slag is aoxidized before mixing with sodium carbonate, is crushed first, make to aoxidize titanium slag
Maximum gauge is not more than 1 millimeter.
In the present embodiment, when being roasted and being calcined, oxygen content is 50%, second in burner hearth for the first step and the 4th step
Step carries out the reducing agent coal gas selected when reduction sodium roasting.
In the present embodiment, in second step, when oxidation titanium slag is mixed with sodium carbonate, sodium carbonate usage amount is that oxidation titanium slag uses
The 40% of amount.
In the present embodiment, inorganic acid is technical hydrochloric acid in third step.
In the present embodiment, the mixed proportion in third step between sodium titanium slag and inorganic acid is：1：12.
In the present embodiment, when third step drying operation, drying temperature is 120 DEG C, and drying time is 2 hours, drying operation
Water content afterwards is not more than 3%.
Embodiment 3
As illustrated in fig. 1 and 2, a method of synthetic rutile is prepared by high calcium magnesium titanium slag, is included the following steps：
The first step, oxidizing roasting carry out 1.2h oxidizing roasting, are aoxidized by high calcium magnesium titanium slag under the conditions of 1000 DEG C of temperature
Titanium slag；
Second step, restore sodium roasting, the oxidation titanium slag and sodium carbonate that the first step is obtained after mixing, at 900 DEG C into
Row 1.5h restores sodium roasting, obtains modified sodium titanium slag；
Third step, acidleach removal of impurities uniformly mix the sodium titanium slag that second step obtains with the inorganic acid that concentration is 20wt%, and
Fluidized state is heated the mixture in 20 minutes and then carries out back flow reaction, then to the residue after back flow reaction in inorganic acid
Middle progress acidleach in 4 hours is finally filtered, washed and is dried to the residue under acidleach state, and acidleach removal of impurities slag is obtained；
4th step, calcining, the acidleach removal of impurities slag that third step is obtained move into crucible, carry out 1.3h under the conditions of 900 DEG C of temperature
Calcining, obtain the synthetic rutile.
In the present embodiment, in the first step, high calcium magnesium titanium slag is not finely ground electro-titanium slag, is chosen between 100 mesh
Particle, wherein+20 mesh particle fraction≤1%, average particle size is 300 μm.
In the present embodiment, high calcium magnesium titanium slag is made of following parts by weight substance in the first step： FeO10wt%,CaO
1.5wt%, MgO 4.5wt%, surplus TiO2.
In the present embodiment, in second step, titanium slag is aoxidized before mixing with sodium carbonate, is crushed first, make to aoxidize titanium slag
Maximum gauge is not more than 1 millimeter.
In the present embodiment, when being roasted and being calcined, oxygen content is 30% in burner hearth for the first step and the 4th step, the
It is coal gas, hydrogen with 1 that two steps, which carry out the reducing agent selected when reduction sodium roasting,：The mixing of 1.5 ratios.
In the present embodiment, in second step, when oxidation titanium slag is mixed with sodium carbonate, sodium carbonate usage amount is that oxidation titanium slag uses
The 30% of amount.
In the present embodiment, inorganic acid is sulfuric acid in third step.
In the present embodiment, the mixed proportion in third step between sodium titanium slag and inorganic acid is：1：10.
In the present embodiment, when third step drying operation, drying temperature is 110 DEG C, and drying time is 1.5 hours, dry to make
Water content after industry is not more than 3%.
Embodiment 4
As illustrated in fig. 1 and 2, titanium slag used is to be produced by the ilmenite of Panzhihua Region by electro-smelting in embodiment
Acid-dissolved titanium slag（20 ~ 160 mesh）, as shown in table 1, X-ray diffraction analysis is shown the main matter composition of the titanium slag（A in Fig. 1）,
The main crystalline structure of the titanium slag is anosovite structure（Main matter group becomes Ti3O5, MgTi2O5 and FeTi2O5）
Specific preparation process is as follows：
High calcium magnesium titanium slag in the present embodiment is placed in Muffle furnace by the first step, oxidizing roasting, empty with 900 DEG C of temperature conditions
2h oxidizing roasting is carried out under gas atmosphere, obtains oxidation titanium slag；
Second step restores sodium roasting, by oxidation titanium slag obtained above and sodium carbonate（The quality of sodium carbonate is the 33% of titanium slag）
After mixing, coal is used（Bituminous coal and anthracite, which are mixed, matches）It as reducing agent, is placed in Muffle furnace, 1h reduction is carried out at 950 DEG C
Sodium roasting carries out very fast cooling after roasting, removes fine particulate coal by washing, obtains modified sodium titanium after dry
Slag.
Third step, acidleach removal of impurities, the sodium titanium slag that second step is obtained and concentration are the inorganic acid of 20wt% in three-necked flask
It is interior uniformly to be mixed by Stirring, liquid-solid ratio 10:1, the back flow reaction 3h under fluidized state carry out acidleach removal of impurities.Reaction
After filtered, washed and dried, obtain acidleach removal of impurities slag；
4th step, calcining, the acidleach removal of impurities slag that third step is obtained move into crucible, carry out 1h's under the conditions of 930 DEG C of temperature
Calcining, obtaining titanium grade is 90.17% synthetic rutile.The specific component of the rutile such as following table：
The chemical substance of titanium slag and its synthetic rutile of preparation forms contrast table
| Sample | TiO2 | TFe | CaO | MgO | S | Al2O3 | SiO2 | MnO |
| Titanium slag（wt%） | 76.21 | 7.01 | 1.76 | 5.78 | 0.17 | 2.39 | 5.58 | 1.10 |
| Synthetic rutile（wt%） | 90.17 | 0.36 | 0.14 | 1.87 | 0.19 | 1.26 | 5.86 | 0 |
Embodiment 5：
As illustrated in fig. 1 and 2, titanium slag used is to be produced by the ilmenite of Panzhihua Region by electro-smelting in embodiment
Acid-dissolved titanium slag（20 ~ 160 mesh）, as shown in table 2, X-ray diffraction analysis is shown the main matter composition of the titanium slag（C in Fig. 1）,
The main crystalline structure of the titanium slag is anosovite structure（Main matter group becomes Ti3O5, MgTi2O5 and FeTi2O5）.
Specific preparation process is as follows：
High calcium magnesium titanium slag in the present embodiment is placed in Muffle furnace by the first step, oxidizing roasting, empty with 950 DEG C of temperature conditions
2h oxidizing roasting is carried out under gas atmosphere, obtains oxidation titanium slag；
Second step restores sodium roasting, by oxidation titanium slag obtained above and sodium carbonate（The quality of sodium carbonate is the 30% of titanium slag）
After mixing, coal is used（Bituminous coal and anthracite, which are mixed, matches）It as reducing agent, is placed in Muffle furnace, 2h reduction is carried out at 1000 DEG C
Sodium roasting carries out very fast cooling after roasting, removes fine particulate coal by washing, obtains modified sodium titanium after dry
Slag.
Third step, acidleach removal of impurities, the sodium titanium slag that second step is obtained and concentration are the inorganic acid of 23wt% in three-necked flask
It is interior uniformly to be mixed by Stirring, liquid-solid ratio 9:1, the back flow reaction 3h under fluidized state carry out acidleach removal of impurities.Reaction knot
It filtered, washed and is dried after beam, obtain acidleach removal of impurities slag；
4th step, calcining, the acidleach removal of impurities slag that third step is obtained move into crucible, carry out 1h's under the conditions of 900 DEG C of temperature
Calcining, obtaining titanium grade is 90.21% synthetic rutile.The specific component of the rutile such as following table：
The chemical substance of titanium slag and its synthetic rutile of preparation forms contrast table
| Sample | TiO2 | TFe | CaO | MgO | S | Al2O3 | SiO2 | MnO |
| Titanium slag（wt%） | 76.21 | 7.01 | 1.76 | 5.78 | 0.17 | 2.39 | 5.58 | 1.10 |
| Synthetic rutile（wt%） | 90.85 | 0.2 | 0.12 | 1.06 | 0.07 | -0.05 | 7.40 | 0 |
Embodiment 6
As illustrated in fig. 1 and 2, titanium slag used is to be produced by the ilmenite of Panzhihua Region by electro-smelting in embodiment
Acid-dissolved titanium slag（20 ~ 160 mesh）, as shown in table 3, X-ray diffraction analysis is shown the main matter composition of the titanium slag（E in Fig. 1）,
The main crystalline structure of the titanium slag is anosovite structure（Main matter group becomes Ti3O5, MgTi2O5 and FeTi2O5）.
Specific preparation process is as follows：
High calcium magnesium titanium slag in the present embodiment is placed in Muffle furnace by the first step, oxidizing roasting, empty with 920 DEG C of temperature conditions
2h oxidizing roasting is carried out under gas atmosphere, obtains oxidation titanium slag；
Second step restores sodium roasting, by oxidation titanium slag obtained above and sodium carbonate（The quality of sodium carbonate is the 34% of titanium slag）
After mixing, coal is used（Bituminous coal and anthracite, which are mixed, matches）It as reducing agent, is placed in Muffle furnace, 2h reduction is carried out at 950 DEG C
Sodium roasting carries out very fast cooling after roasting, removes fine particulate coal by washing, obtains modified sodium titanium after dry
Slag.
Third step, acidleach removal of impurities, the sodium titanium slag that step B is obtained and concentration are the inorganic acid of 19wt% in three-necked flask
It is interior uniformly to be mixed by Stirring, liquid-solid ratio 10:1, the back flow reaction 4h under fluidized state carry out acidleach removal of impurities.Reaction
After filtered, washed and dried, obtain acidleach removal of impurities slag；
4th step, calcining, the acidleach removal of impurities slag that step C is obtained move into crucible, carry out 1h's under the conditions of 900 DEG C of temperature
Calcining, obtaining titanium grade is 91.45% synthetic rutile.The specific component of the rutile such as following table：
The chemical substance of titanium slag and its synthetic rutile of preparation forms contrast table
| Sample | TiO2 | TFe | CaO | MgO | S | Al2O3 | SiO2 | MnO |
| Titanium slag（wt%） | 75.65 | 12.08 | 1.15 | 5.19 | 0.21 | 1.99 | 4.00 | 1.49 |
| Synthetic rutile（wt%） | 91.45 | 0.37 | 0.12 | 1.13 | 0.16 | 1.01 | 5.20 | 0.08 |
The present invention handles high calcium magnesium titanium slag by the way of oxidizing roasting-reduction sodium roasting-acidleach-calcining, to impurity element
The removal effect of Fe, Ca, Mg are preferable, and obtained synthetic rutile titanium grade is higher.Firstly, reduction phase be added sodium carbonate into
Row sodium roasting, anosovite structure destroy ratio more thoroughly, conducive to the removal of impurity when subsequent acidleach；Secondly, and due to reduction
There is the presence of reducing agent in stage（Such as coal）, keep material loose porous, the sintering phenomenon of firing stage can be mitigated to a certain degree.
Meanwhile when restoring sodium roasting, if the dosage of sodium carbonate is more than this range, black titanium cannot be destroyed well
The structure of stone, and then also it is unfavorable for the removal of impurity when acidleach, the additive amount of sodium carbonate is preferably the 25 ~ 35% of titanium slag.If carbon
The dosage of sour sodium is lower than this range, then the meeting that anosovite structure is destroyed is not thorough enough, causes rutile titanium grade lower；Roasting
If the dosage of sodium carbonate is higher than this range, the sintering phenomenon of sodium roasting product will lead to than more serious.
High calcium magnesium titanium slag-oxidizing roasting of the invention-reduction sodium roasting-acidleach removal of impurities-calcining technique, can be effective
Raising impurity removal rate, promote the titanium grade of synthetic rutile.The preparation method of synthetic rutile of the present invention can
It is widely used in that the electro-titanium slag of the impurity elements such as calcium and magnesium can not be effectively removed by general traditional handicraft, is particularly suitable for climbing
Branch spends the high calcium magnesium titanium slag of regional ilmenite production.In the process of the invention, it is not needed after titanium slag used is broken further thin
Mill saves labour, reduces equipment and uses.In the process of the invention, oxidizing roasting makes a part of anosovite be changed into golden red
Stone structure, and then make the more thorough of anosovite structure destruction in the reduction sodium roasting stage.And reduction phase Fe3+ is basic
It is changed into Fe2+, is more advantageous to next step acidleach removal of impurities.In the process of the invention, acid leaching stage can be with industrial waste acid come generation
It replaces, realizes waste utilization.Rutile preparation method of the invention can be used to handle high calcium magnesium titanium slag, the low, calcium and magnesium by titanium grade
The high electro-titanium slag of content makes full use of, and obtains the raw material-synthetic rutile for being able to satisfy fluidizing chlorination requirement.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (9)
1. a kind of method for preparing synthetic rutile by high calcium magnesium titanium slag, it is characterised in that：Described is prepared by high calcium magnesium titanium slag
The method of synthetic rutile includes the following steps：
The first step, oxidizing roasting carry out 1 ~ 2h oxidizing roasting, obtain by high calcium magnesium titanium slag under the conditions of 900 DEG C ~ 1050 DEG C of temperature
To oxidation titanium slag；
Second step, restore sodium roasting, the oxidation titanium slag and sodium carbonate that the first step is obtained after mixing, 850 DEG C ~ 1000
1 ~ 2h is carried out at DEG C and restores sodium roasting, obtains modified sodium titanium slag；
Third step, acidleach removal of impurities uniformly mix the sodium titanium slag that second step obtains with the inorganic acid that concentration is 15 ~ 25wt%, and
Fluidized state is heated the mixture in 10-30 minutes and then carries out back flow reaction, is then existed to the residue after back flow reaction
Acidleach in 3-5 hours is carried out in inorganic acid, and finally the residue under acidleach state is filtered, washed and dried, obtains acid
The miscellaneous slag of leaching；
4th step, calcining, the acidleach removal of impurities slag that third step is obtained moves into crucible, under the conditions of 850 DEG C ~ 1000 DEG C of temperature
The calcining for carrying out 1 ~ 2h obtains the synthetic rutile.
2. a kind of method for preparing synthetic rutile by high calcium magnesium titanium slag according to claim 1, which is characterized in that first
In step, high calcium magnesium titanium slag is not finely ground electro-titanium slag, the particle between 20 ~ 160 mesh is chosen, wherein+20 mesh particle ratios
Example≤1%, average particle size are 250 ~ 500 μm.
3. a kind of method for preparing synthetic rutile by high calcium magnesium titanium slag according to claim 1, which is characterized in that first
High calcium magnesium titanium slag is made of following parts by weight substance in step：FeO7 ~ 13wt%, 1 ~ 2wt% of CaO, 3 ~ 6wt% of MgO, surplus are
TiO2 。
4. a kind of method for preparing synthetic rutile by high calcium magnesium titanium slag according to claim 1, which is characterized in that second
In step, titanium slag is aoxidized before mixing with sodium carbonate, is crushed first, make to aoxidize titanium slag maximum gauge no more than 1 millimeter.
5. a kind of method for preparing synthetic rutile by high calcium magnesium titanium slag according to claim 1, which is characterized in that first
When being roasted and being calcined, oxygen content is not less than 21% in burner hearth, and second step carries out reduction sodium roasting for step and the 4th step
The reducing agent of Shi Xuanyong is that one of coal, coal gas, hydrogen, petroleum coke or any two kinds are mixed with arbitrary proportion.
6. a kind of method for preparing synthetic rutile by high calcium magnesium titanium slag according to claim 1, which is characterized in that second
In step, when oxidation titanium slag is mixed with sodium carbonate, sodium carbonate usage amount is aoxidize titanium slag usage amount 20-40%.
7. a kind of method for preparing synthetic rutile by high calcium magnesium titanium slag according to claim 1, which is characterized in that third
Inorganic acid is any one in technical hydrochloric acid or sulfuric acid in step.
8. a kind of method for preparing synthetic rutile by high calcium magnesium titanium slag according to claim 1, which is characterized in that third
Mixed proportion in step between sodium titanium slag and inorganic acid is：1：8—12.
9. a kind of method for preparing synthetic rutile by high calcium magnesium titanium slag according to claim 1, which is characterized in that third
When walking drying operation, drying temperature is 100-120 DEG C, and drying time is 1-2 hours, and the water content after drying operation is not more than
3%。
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