CN107399758A - A kind of method that synthetic rutile is prepared by high titanium slag - Google Patents
A kind of method that synthetic rutile is prepared by high titanium slag Download PDFInfo
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- CN107399758A CN107399758A CN201610338055.2A CN201610338055A CN107399758A CN 107399758 A CN107399758 A CN 107399758A CN 201610338055 A CN201610338055 A CN 201610338055A CN 107399758 A CN107399758 A CN 107399758A
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to a kind of method that synthetic rutile is prepared by high titanium slag, this method includes the steps such as high titanium slag crushes, alkali leaching is miscellaneous, modified roasting, acid removal of impurities and calcining.This method improves heating rate and heating effect, while more traditional roasting is compared, and reduces energy consumption of reaction using microwave as thermal source；The sintering temperature of high titanium slag reduces, and roasting technique becomes simple, both ensured the grade of titanium dioxide, so as to get synthetic rutile meet that chloridising produces titanium white, substantially reduce the production cycle again, reduce production cost.Meanwhile combined using soda acid and leached, the impurity in high titanium slag, such as calcium oxide, aluminum oxide, silica are also effectively removes, also greatly improves the grade of rutile.
Description
Technical field
The present invention relates to a kind of method that synthetic rutile is prepared by high titanium slag, belong to microwave metallurgical technical field.
Background technology
High titanium slag is the product of slag sluicing system after ilmenite electric furnace reduction melting, as the high-quality of production synthetic rutile
Raw material.With the development of Ti industry, natural rutile resource is petered out, it is felt to be desirable to is enriched with rich-titanium material.Synthetic rutile
Be on composition and structural behaviour with natural rutile identical rich-titanium material, be natural rutile high-quality substitute, can be used for
Chloridising produces titanium white.The production method of synthetic rutile includes electrothermal way, Reductive leaching and the acid-hatching of young eggs at present.
Traditional heating roasting high titanium slag firing rate is slow, heats uneven, high energy consumption.With to the increasingly heavy of the utilization of resources
Depending on developing the production technology of energy-saving roasting high titanium slag, turning into irresistible trend.Microwave heating is to grow up in recent years
A kind of New Metallurgical Technique, there is internal heating, quick heating is easily controllable, the features such as energy-conservation.Using microwave calcining-soda acid
The method that joint leaches high titanium slag, production efficiency can not only be greatly improved, reduce energy consumption, and after soda acid leaching, wherein
Impurity can effectively remove, obtain high-grade synthetic rutile.
Number of patent application is " 201010170363.1 ", and entitled " a kind of method of producing synthetic rutile by using titania slag " proposes
The titanium slag that one kind is melted out with electric furnace, blast furnace etc. is artificial being prepared by alkali roasting-water washing-hydrochloric acid extract technology for raw material
The method of rutile.After titanium slag is mixed with alkali, it is calcined, product of roasting carries out multi-stage countercurrent washing, separation of solid and liquid, washing
Product carries out leaching removal of impurities with dilute hydrochloric acid solution afterwards, then will leach solid-liquid separation on ore pulp, and wash heat is washed, and dries, and calcining prepares artificial
Rutile.The advantages of method is that the impurity such as calcium and magnesium aluminium removal rate is high and product content of titanium dioxide is high, realizes alkali circulation and salt
The regeneration of acid.But the shortcomings that method is that roasting process heating rate is slow, calcination process time length, the production cycle is caused
It is long, high energy consumption.
The content of the invention
Technical problems to be solved]
It is an object of the invention to provide a kind of method that synthetic rutile is prepared by high titanium slag.
Technical scheme]
The present invention is realized by following proposal.
The present invention relates to a kind of method that synthetic rutile is prepared by high titanium slag.
The step of preparation method, is as follows.
A, crush
High titanium slag is ground to -100 mesh by weight more than 80% using milling apparatus first, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 20 ~ 40% aqueous slkali according to solid-to-liquid ratio 1:5 ~ 8 is well mixed,
It is placed in water-bath and carries out miscellaneous 60 ~ 120 min of alkali leaching at boiling temperature；Then filtered, washed and dried, obtain alkali
The miscellaneous slag of leaching, then
C, modified roasting
Carried out sodium carbonate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 20 ~ 40% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is carried out in microwave device under conditions of 700 ~ 900 DEG C micro-
Wavefront modifier is calcined, and obtains a kind of modified titanium-rich slag, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 20 ~ 30% inorganic acid with solid-to-liquid ratio 1:4 ~ 6 is well mixed,
It is placed in water-bath and carries out 60 ~ 120 min of acidleach removal of impurities at boiling temperature.Then filtered, washed and dried, obtain acid
The miscellaneous slag of leaching, then
E, calcine
Acidleach that step D is obtained removal of impurities slag is put into crucible, is placed in microwave device in the temperature strip of 900 ~ 1000 DEG C of temperature
Calcined under part, obtain the synthetic rutile.
A preferred embodiment of the invention, in step, the high titanium slag are TiO by weight2Content is
More than 85.0%, SiO2For less than 4.0% titanium slag.
According to another preferred embodiment of the present invention, in stepb, the aqueous slkali is sodium hydroxide solution.
According to the present invention another preferred embodiment, in stepb, the sodium carbonate liquor modifying agent can use sodium sulphate or
Phosphate replaces.
According to another preferred embodiment of the present invention, in step C, the microwave irradiation time is 30 ~ 60 min.
According to another preferred embodiment of the present invention, in step C, the frequency of the microwave device for 2350 ~
2450MHz。
According to another preferred embodiment of the present invention, microwave heating is controlled to rise in step C, during the microwave calcining
Warm speed is 10 ~ 100 DEG C/min.
According to another preferred embodiment of the present invention, in step D, the inorganic acid is sulfuric acid or hydrochloric acid.
According to another preferred embodiment of the present invention, in step E, the calcining is in frequency in microwave device
20 ~ 40 min are handled under conditions of 2350 ~ 2450MHz.
According to another preferred embodiment of the present invention, the purity of the synthetic rutile is by weight more than 91%.
The present invention is described in more detail below.
Brief description of the drawings
Fig. 1 is the x-ray diffraction pattern of the rutile prepared using the inventive method.
Embodiment
The present invention relates to a kind of method that synthetic rutile is prepared by high titanium slag.
The present invention just uses microwave calcining-soda acid Combined Treatment high titanium slag.First, this method improves using microwave as thermal source
Heating rate and heating effect, while microwave irradiation processing can make to produce obvious intercrystalline crackle inside high titanium slag, after being easy to
Continuous leaching agent enters high titanium slag, it is easier to leaches.Leached second, being combined using soda acid, effectively eliminate the impurity in high titanium slag,
Improve grade of titanium dioxide.
The step of preparation method, is as follows：
A, crush
High titanium slag is ground to -100 mesh by weight more than 80% using milling apparatus first, obtains a kind of high titanium slag powder.
The high titanium slag that the present invention uses is the product of slag sluicing system after ilmenite electro-smelting.TiO by weight2Content
More than 85%, SiO2Below 4.0%.
Wherein, TiO2Content be to be determined according to GB/T1706-2006 standards using aluminum reduction method.SiO2It is according to YB/
T190.1-2001 standards are using perchloric acid determination measure.
In the present invention, it is ground and sieves with screening plant using existing pulverising apparatus, for example, it is general by Nanchang
Analysis and sample making factory is with trade name sealed type sample pulverizer（JG100-3）The pulverising apparatus of sale, by Zhejiang Shangyu city road ruins five
The screening plant that four instrument plants are sold with trade name standard screen.
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 20 ~ 40% aqueous slkali according to solid-to-liquid ratio 1:5 ~ 8 is well mixed,
It is placed in water-bath and carries out miscellaneous 60 ~ 120 min of alkali leaching at boiling temperature；Then filtered, washed and dried, obtain alkali
The miscellaneous slag of leaching.
In the present invention, described aqueous slkali be concentration by weight 20 ~ 40% sodium hydroxide solution, SiO can be removed2
Impurity.
In this step, if the concentration of the aqueous slkali exceedes this scope, it can not well reach and clean
The purpose of matter.Alkali concn is preferably 22 ~ 28%, more preferably 25 ~ 35%.
According to the present invention, if the solid-to-liquid ratio of high titanium slag and aqueous slkali is higher than 1:5, then leaching agent can be made to quickly reach saturation
Degree so that leach incomplete；If the solid-to-liquid ratio of high titanium slag and aqueous slkali is less than 1:8, then it can increase the consumption of alkali, and be not easy to grasp
Make；Therefore, the solid-to-liquid ratio of high titanium slag and aqueous slkali is 1:5 ~ 8 be it is suitable, preferably 1:5.5, more preferably 1:6~1:
7.5。
In this step, the miscellaneous equipment of alkali leaching is thermostat water bath, by Yu Hua Instrument Ltd. of Gongyi City with business
Name of an article constant-temperature heating magnetic stirring apparatus（DF-101S）The thermostat water bath of sale.
In this step, equipment used during filtering is current market sales of product, such as plum Teller-towing force is more
Instrument Ltd. is with trade name circulating water type vavuum pump（SHZ-D(Ⅲ)）The product of sale.
The drying equipment that the present invention uses is current market sales of product, for example, Shanghai it is rich prove to be true after interrogation industry equipment company with
Trade name digital display air dry oven（DZX-9030MBE）The product of sale.
C, modified roasting
Carried out sodium carbonate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 20 ~ 40% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is carried out in microwave device under conditions of 700 ~ 900 DEG C micro-
Wavefront modifier is calcined, and obtains a kind of modified titanium-rich slag.
In the present invention, described modification is it should be understood that a kind of processing for changing high titanium slag thing phase composition.
In the present invention, described modifying agent is it should be understood that a kind of have the chemicals for destroying solid solution structure ability
Matter, it is therefore, every that there is this property, and there is no other dysgenic chemical substances to may be used to this to subsequent treatment
Invention, also within protection scope of the present invention.
In addition to modification of sodium carbonate agent, modifying agent of the invention can also use sodium sulphate or phosphate to replace.
In the present invention, if the amount of the modifying agent is less than 20%, it can react incomplete, have part high titanium slag not
Realize reaction；If the amount of the modifying agent is higher than 40%, the modifying agent unreacted of part is had, consumes excessive modifying agent；
Therefore, the amount of the modifying agent be 20% ~ 40% be it is rational, preferably 22% ~ 38%；More preferably 30% ~ 36%.
The high titanium slag need to carry out microwave sodium roasting modification 30 ~ 60 with modifying agent under conditions of 700 ~ 900 DEG C
min。
The high titanium slag microwave calcining temperature is less than 700 DEG C, then can react insufficient；Treatment temperature is higher than 900 DEG C, then can
There is sintering phenomenon, while cause unnecessary energy consumption；Then the temperature of microwave calcining processing is reasonable for 700 DEG C ~ 900 DEG C
, preferably 750 DEG C ~ 850 DEG C.
Likewise, if microwave calcining processing time is less than 30 min, can react incomplete；Processing time is longer than 60
Min, then it can produce unnecessary energy expenditure；Therefore, microwave calcining processing time be 30 ~ 60 min be it is rational, preferably
It is 35 ~ 57 min, more preferably 40 ~ 55 min.
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 20 ~ 30% inorganic acid with solid-to-liquid ratio 1:4 ~ 6 is well mixed,
It is placed in water-bath and carries out 60 ~ 120 min of acidleach removal of impurities at boiling temperature.Then filtered, washed and dried, obtain acid
The miscellaneous slag of leaching.
In this step, the inorganic acid uses sulfuric acid or hydrochloric acid, can remove such as Fe2O3、CaO、MgO、Al2O3Deng
Impurity.
According to the present invention, if the solid-to-liquid ratio of modified slag and inorganic acid is higher than 1:4, then it can leach slag specimen incomplete；Such as
Fruit is modified slag and the solid-to-liquid ratio of inorganic acid is less than 1:6, then it can increase the dosage of inorganic acid, and meanwhile it is not easy to operate.Therefore, modified slag
Solid-to-liquid ratio with inorganic acid is 1:4 ~ 6 be it is feasible, preferably 1:4.5 ~ 5.5, more preferably 1:4.8~5.8.
In this step, acidleach, if extraction time is less than 30 min, can react except miscellaneous time is 60 ~ 120 min
Not exclusively；Extraction time is longer than 60 min, then can produce unnecessary energy expenditure；Therefore, it is 60 ~ 120 that acidleach, which removes miscellaneous time,
Min is rational, preferably 65 ~ 105min, more preferably 80 ~ 100 min.
In this step, equipment used in acidleach removal of impurities is thermostat water bath, is given by Gongyi City
Magnificent Instrument Ltd. is with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The thermostat water bath of sale.
In this step, equipment used during filtering is current market sales of product, such as plum Teller-towing force is more
Instrument Ltd. is with trade name circulating water type vavuum pump（SHZ-D(Ⅲ)）The product of sale.
The drying equipment that the present invention uses is current market sales of product, for example, Shanghai it is rich prove to be true after interrogation industry equipment company with
Trade name digital display air dry oven（DZX-9030MBE）The product of sale.
E, calcine
Acidleach that step D is obtained removal of impurities slag is put into crucible, is placed in microwave device in the temperature strip of 900 ~ 1000 DEG C of temperature
Calcined under part, obtain the synthetic rutile.
It is to handle 20 ~ 40 min under conditions of 2350 ~ 2450MHz of frequency in microwave device in this calcining step.
According to the present invention, if calcining heat is less than 900 DEG C, the anatase titanium dioxide TiO of part2Crystal formation does not occur to turn completely
Become；If temperature is higher than 1000 DEG C, sintering phenomenon occurs, while cause unnecessary energy consumption；Therefore, calcining heat is
900 ~ 1000 DEG C are appropriate, preferably 920 ~ 980 DEG C, more preferably 940 ~ 960 DEG C.
In this calcining step, obtained product has carried out X-ray diffraction structure qualitative analysis.
Equipment used in X-ray diffraction analysis is the X-ray diffraction analysis instrument of Japanese Rigaku companies（D/
Max2200X）, analysis condition is pipe pressure 35Kv, pipe stream 20mA, and~2 θ step-scan modes are filtered, θ using graphite monochromator,
Analysis test is carried out with 3 °/min sweep speed in the range of 3 ~ 100 °.
X-ray diffraction analysis result is listed in accompanying drawing 1.By accompanying drawing 1 it was determined that the product that calcining step obtains is rutile.
Beneficial effect]
The beneficial effects of the invention are as follows：Compared with prior art, the inventive method is using microwave as thermal source, improve heating rate and
Heating effect, while more traditional roasting is compared, and reduces energy consumption of reaction；This method causes the sintering temperature of high titanium slag to reduce, roasting
Firing technique becomes simple, has both ensured the grade of titanium dioxide, so as to get synthetic rutile meet that chloridising produces titanium white, and greatly
The production cycle is shortened greatly, reduces production cost；The inventive method is leached using soda acid joint, and impurity therein can be effective
Remove, can obtain more than 91% high-grade artificial rutile.
Embodiment
The present invention is will be better understood that by following embodiments.
Embodiment 1：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 85.5%,
SiO23.94%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 22% sodium hydroxide solution according to solid-to-liquid ratio 1:5.5 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 60 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 100 DEG C of temperature
60 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out sodium carbonate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 23% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in Kunming University of Science and Technology with the box reactor of trade name microwave
（HM types）In the microwave device of sale, microwave sodium modification roasting is carried out under conditions of frequency is 2350MHz and temperature is 750 DEG C
Burn, control heating rate is in 70 DEG C/min, and after temperature reaches 750 DEG C, the min of soaking time 35 obtains the modification of microwave sodium roasting
High titanium slag, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 22% sulfuric acid with solid-to-liquid ratio 1:4.5 is well mixed, then
Using by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The water bath with thermostatic control of sale
Pot carries out acidleach removal of impurities 70 min of processing, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name circulating water type
Vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with trade name
Digital display air dry oven（DZX-9030MBE）60 min are dried under conditions of 100 DEG C of temperature in the drying equipment of sale, obtain
To the miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2350MHz and temperature is 920 DEG C
Heating rate is in 70 DEG C/min, after temperature reaches 920 DEG C, the min of soaking time 20, obtains described 91.3% synthetic rutile.
Embodiment 2：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 86.3%,
SiO23.87%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 25% sodium hydroxide solution according to solid-to-liquid ratio 1:6 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 90 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 105 DEG C of temperature
60 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out sodium carbonate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 25% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in Kunming University of Science and Technology with the box reactor of trade name microwave
（HM types）In the microwave device of sale, microwave sodium modification roasting is carried out under conditions of frequency is 2355MHz and temperature is 800 DEG C
Burn, control heating rate is in 75 DEG C/min, and after temperature reaches 800 DEG C, the min of soaking time 45 obtains the modification of microwave sodium roasting
High titanium slag, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 25% sulfuric acid with solid-to-liquid ratio 1:4.8 is well mixed, then
Using by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The water bath with thermostatic control of sale
Pot carries out acidleach removal of impurities 90 min of processing, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name circulating water type
Vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with trade name
Digital display air dry oven（DZX-9030MBE）60 min are dried under conditions of 105 DEG C of temperature in the drying equipment of sale, obtain
To the miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2355MHz and temperature is 940 DEG C
Heating rate is in 75 DEG C/min, after temperature reaches 940 DEG C, the min of soaking time 30, obtains described 91.8% synthetic rutile.
Embodiment 3：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 86.7%,
SiO23.62%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 30% sodium hydroxide solution according to solid-to-liquid ratio 1:7 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 90 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 100 DEG C of temperature
70 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out sodium carbonate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 30% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in Kunming University of Science and Technology with the box reactor of trade name microwave
（HM types）In the microwave device of sale, microwave sodium modification roasting is carried out under conditions of frequency is 2400MHz and temperature is 900 DEG C
Burn, control heating rate is in 65 DEG C/min, and after temperature reaches 900 DEG C, the min of soaking time 50 obtains the modification of microwave sodium roasting
High titanium slag, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 30% sulfuric acid with solid-to-liquid ratio 1:5 is well mixed, then makes
With by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The thermostat water bath of sale
Acidleach removal of impurities 100 min of processing are carried out, are then used true with trade name circulating water type by plum Teller-towing force multiple instruments Co., Ltd
Empty pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with commodity concrete number
Aobvious air dry oven（DZX-9030MBE）70 min are dried under conditions of 100 DEG C of temperature in the drying equipment of sale, obtain
The miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2400MHz and temperature is 950 DEG C
Heating rate is in 65 DEG C/min, after temperature reaches 950 DEG C, the min of soaking time 40, obtains described 92.2% synthetic rutile.
Embodiment 4：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 85.9%,
SiO23.75%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 35% sodium hydroxide solution according to solid-to-liquid ratio 1:8 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 120 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 105 DEG C of temperature
60 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out sodium carbonate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 35% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in Kunming University of Science and Technology with the box reactor of trade name microwave
（HM types）In the microwave device of sale, microwave sodium modification roasting is carried out under conditions of frequency is 2450MHz and temperature is 850 DEG C
Burn, control heating rate is in 80 DEG C/min, and after temperature reaches 850 DEG C, the min of soaking time 60 obtains the modification of microwave sodium roasting
High titanium slag, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 25% sulfuric acid with solid-to-liquid ratio 1:6 is well mixed, then makes
With by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The thermostat water bath of sale
Acidleach removal of impurities 120 min of processing are carried out, are then used true with trade name circulating water type by plum Teller-towing force multiple instruments Co., Ltd
Empty pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with commodity concrete number
Aobvious air dry oven（DZX-9030MBE）60 min are dried under conditions of 105 DEG C of temperature in the drying equipment of sale, obtain
The miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2450MHz and temperature is 1000 DEG C
Heating rate is in 80 DEG C/min, after temperature reaches 1000 DEG C, the min of soaking time 30, obtains described 92.8% synthetic rutile.
Embodiment 5：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 86.8%,
SiO23.51%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 35% sodium hydroxide solution according to solid-to-liquid ratio 1:6 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 90 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 100 DEG C of temperature
60 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out sodium sulphate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 30% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in Kunming University of Science and Technology with the box reactor of trade name microwave
（HM types）In the microwave device of sale, microwave sodium modification roasting is carried out under conditions of frequency is 2450MHz and temperature is 850 DEG C
Burn, control heating rate is in 75 DEG C/min, and after temperature reaches 750 DEG C, the min of soaking time 45 obtains the modification of microwave sodium roasting
High titanium slag, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 25% hydrochloric acid with solid-to-liquid ratio 1:6 is well mixed, then makes
With by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The thermostat water bath of sale
Acidleach removal of impurities 90 min of processing are carried out, are then used true with trade name circulating water type by plum Teller-towing force multiple instruments Co., Ltd
Empty pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with commodity concrete number
Aobvious air dry oven（DZX-9030MBE）60 min are dried under conditions of 100 DEG C of temperature in the drying equipment of sale, obtain
The miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2450MHz and temperature is 950 DEG C
Heating rate is in 75 DEG C/min, after temperature reaches 950 DEG C, the min of soaking time 30, obtains described 91.7% synthetic rutile.
Embodiment 6：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 85.2%,
SiO23.96%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 35% sodium hydroxide solution according to solid-to-liquid ratio 1:7 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 120 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 105 DEG C of temperature
60 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out disodium-hydrogen is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is that alkali leaching is miscellaneous
The 35% of slag weight, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in Kunming University of Science and Technology with the box reaction of trade name microwave
Device（HM types）In the microwave device of sale, microwave sodium modification is carried out under conditions of frequency is 2450MHz and temperature is 850 DEG C
Roasting, control heating rate is in 70 DEG C/min, and after temperature reaches 850 DEG C, the min of soaking time 60 obtains microwave sodium roasting and changed
Property high titanium slag, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 28% sulfuric acid with solid-to-liquid ratio 1:5 is well mixed, then makes
With by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The thermostat water bath of sale
Acidleach removal of impurities 120 min of processing are carried out, are then used true with trade name circulating water type by plum Teller-towing force multiple instruments Co., Ltd
Empty pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with commodity concrete number
Aobvious air dry oven（DZX-9030MBE）60 min are dried under conditions of 105 DEG C of temperature in the drying equipment of sale, obtain
The miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2450MHz and temperature is 960 DEG C
Heating rate is in 70 DEG C/min, after temperature reaches 960 DEG C, the min of soaking time 40, obtains described 92.4% synthetic rutile.
Comparative example 1：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 85.5%,
SiO23.94%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 22% sodium hydroxide solution according to solid-to-liquid ratio 1:5.5 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 60 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 100 DEG C of temperature
60 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out sodium carbonate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 23% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in resistance furnace and is carried out sodium under conditions of 750 DEG C of temperature
Modified roasting, control heating rate is in 70 DEG C/min, and after temperature reaches 750 DEG C, the min of soaking time 35 obtains the roasting of microwave sodium
Modified titanium-rich slag is burnt, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 22% sulfuric acid with solid-to-liquid ratio 1:4.5 is well mixed, then
Using by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The water bath with thermostatic control of sale
Pot carries out acidleach removal of impurities 70 min of processing, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name circulating water type
Vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with trade name
Digital display air dry oven（DZX-9030MBE）60 min are dried under conditions of 100 DEG C of temperature in the drying equipment of sale, obtain
To the miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2350MHz and temperature is 920 DEG C
Heating rate is in 70 DEG C/min, after temperature reaches 920 DEG C, the min of soaking time 20, obtains described 80.14% synthetic rutile.
Comparative example 2：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 86.3%,
SiO23.87%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 25% sodium hydroxide solution according to solid-to-liquid ratio 1:6 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 90 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 105 DEG C of temperature
60 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out sodium carbonate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 25% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in resistance furnace and is carried out sodium under conditions of 800 DEG C of temperature
Modified roasting, control heating rate is in 75 DEG C/min, and after temperature reaches 800 DEG C, the min of soaking time 45 obtains the roasting of microwave sodium
Modified titanium-rich slag is burnt, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 25% sulfuric acid with solid-to-liquid ratio 1:4.8 is well mixed, then
Using by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The water bath with thermostatic control of sale
Pot carries out acidleach removal of impurities 90 min of processing, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name circulating water type
Vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with trade name
Digital display air dry oven（DZX-9030MBE）60 min are dried under conditions of 105 DEG C of temperature in the drying equipment of sale, obtain
To the miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2355MHz and temperature is 940 DEG C
Heating rate is in 75 DEG C/min, after temperature reaches 940 DEG C, the min of soaking time 30, obtains described 79.21% synthetic rutile.
Comparative example 3：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 86.7%,
SiO23.62%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 30% sodium hydroxide solution according to solid-to-liquid ratio 1:7 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 90 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 100 DEG C of temperature
70 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out sodium carbonate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 30% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in resistance furnace and is carried out sodium under conditions of 900 DEG C of temperature
Modified roasting, control heating rate is in 65 DEG C/min, and after temperature reaches 900 DEG C, the min of soaking time 50 obtains the roasting of microwave sodium
Modified titanium-rich slag is burnt, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 30% sulfuric acid with solid-to-liquid ratio 1:5 is well mixed, then makes
With by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The thermostat water bath of sale
Acidleach removal of impurities 100 min of processing are carried out, are then used true with trade name circulating water type by plum Teller-towing force multiple instruments Co., Ltd
Empty pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with commodity concrete number
Aobvious air dry oven（DZX-9030MBE）70 min are dried under conditions of 100 DEG C of temperature in the drying equipment of sale, obtain
The miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2400MHz and temperature is 950 DEG C
Heating rate is in 65 DEG C/min, after temperature reaches 950 DEG C, the min of soaking time 40, obtains described 76.84% synthetic rutile.
Comparative example 4：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 85.9%,
SiO23.75%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 35% sodium hydroxide solution according to solid-to-liquid ratio 1:8 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 120 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 105 DEG C of temperature
60 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out sodium carbonate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 35% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in resistance furnace and is carried out sodium under conditions of 850 DEG C of temperature
Modified roasting, control heating rate is in 80 DEG C/min, and after temperature reaches 850 DEG C, the min of soaking time 60 obtains the roasting of microwave sodium
Modified titanium-rich slag is burnt, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 25% sulfuric acid with solid-to-liquid ratio 1:6 is well mixed, then makes
With by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The thermostat water bath of sale
Acidleach removal of impurities 120 min of processing are carried out, are then used true with trade name circulating water type by plum Teller-towing force multiple instruments Co., Ltd
Empty pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with commodity concrete number
Aobvious air dry oven（DZX-9030MBE）60 min are dried under conditions of 105 DEG C of temperature in the drying equipment of sale, obtain
The miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2450MHz and temperature is 1000 DEG C
Heating rate is in 80 DEG C/min, after temperature reaches 1000 DEG C, the min of soaking time 30, obtains described 82.06% artificial golden red
Stone.
Comparative example 5：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 86.8%,
SiO23.51%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 35% sodium hydroxide solution according to solid-to-liquid ratio 1:6 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 90 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 100 DEG C of temperature
60 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out sodium sulphate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching
The 30% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in resistance furnace and is carried out sodium under conditions of 850 DEG C of temperature
Modified roasting, control heating rate is in 75 DEG C/min, and after temperature reaches 750 DEG C, the min of soaking time 45 obtains the roasting of microwave sodium
Modified titanium-rich slag is burnt, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 25% hydrochloric acid with solid-to-liquid ratio 1:6 is well mixed, then makes
With by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The thermostat water bath of sale
Acidleach removal of impurities 90 min of processing are carried out, are then used true with trade name circulating water type by plum Teller-towing force multiple instruments Co., Ltd
Empty pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with commodity concrete number
Aobvious air dry oven（DZX-9030MBE）60 min are dried under conditions of 100 DEG C of temperature in the drying equipment of sale, obtain
The miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2450MHz and temperature is 950 DEG C
Heating rate is in 75 DEG C/min, after temperature reaches 950 DEG C, the min of soaking time 30, obtains described 80.18% synthetic rutile.
Comparative example 6：The preparation of synthetic rutile
The implementation steps of the embodiment are as follows：
A, crush
The method described using this specification has carried out chemical analysis to high titanium slag, its TiO2Content is by weight 85.2%,
SiO23.96%.Using by Nanchang it is general chemical examination sampling machine factory with trade name sealed type sample pulverizer（JG100-3）Sale
High titanium slag is ground to -100 mesh as by weight more than 80% by milling apparatus, obtains a kind of high titanium slag powder, then
B, alkali leaching is miscellaneous
High titanium slag powder that step A is obtained and concentration by weight 35% sodium hydroxide solution according to solid-to-liquid ratio 1:7 mixing are equal
It is even, then use by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）Sale
Thermostat water bath carries out alkali leaching and lives together 120 min of reason, then uses by plum Teller-towing force multiple instruments Co., Ltd with trade name
Circulating water type vavuum pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich
With trade name digital display air dry oven（DZX-9030MBE）The drying equipment of sale is dried under conditions of 105 DEG C of temperature
60 min, the miscellaneous slag of alkali leaching is obtained, then
C, modified roasting
Carried out disodium-hydrogen is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is that alkali leaching is miscellaneous
The 35% of slag weight, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is placed in resistance furnace under conditions of 850 DEG C of temperature and carries out
Sodium modification is calcined, and control heating rate is in 70 DEG C/min, and after temperature reaches 850 DEG C, the min of soaking time 60 obtains microwave sodium
Change modification by calcination high titanium slag, then
D, acidleach cleans
Modified titanium-rich slag that step C is obtained and concentration by weight 28% sulfuric acid with solid-to-liquid ratio 1:5 is well mixed, then makes
With by Yu Hua Instrument Ltd. of Gongyi City with trade name constant-temperature heating magnetic stirring apparatus（DF-101S）The thermostat water bath of sale
Acidleach removal of impurities 120 min of processing are carried out, are then used true with trade name circulating water type by plum Teller-towing force multiple instruments Co., Ltd
Empty pump（SHZ-D(Ⅲ)）The filter plant of sale is filtered, and is reused and is proved to be true after interrogation industry equipment company by Shanghai is rich with commodity concrete number
Aobvious air dry oven（DZX-9030MBE）60 min are dried under conditions of 105 DEG C of temperature in the drying equipment of sale, obtain
The miscellaneous slag of alkali leaching, then
E, calcine
The acidleach removal of impurities slag that step D is obtained is put into crucible, in Kunming University of Science and Technology with the box reactor of trade name microwave（HM
Type）Microwave calcination processing, control are carried out in the microwave device of sale under conditions of frequency is 2450MHz and temperature is 960 DEG C
Heating rate is in 70 DEG C/min, after temperature reaches 960 DEG C, the min of soaking time 40, obtains described 78.06% synthetic rutile.
The embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula, in those of ordinary skill in the art's possessed knowledge, it can also make on the premise of present inventive concept is not departed from
Various change.The result of implementation of embodiment 1 ~ 6 and the result of implementation comparative analysis of comparative example 1 ~ 6 are pointed out, using the present invention
The synthetic rutile purity that method obtains is higher than comparative example by 15.36%.This result be beyond expectations outside knot
Fruit.
Claims (10)
- A kind of 1. method that synthetic rutile is prepared by high titanium slag, it is characterised in that comprise the following steps that：A, crushHigh titanium slag is ground to -100 mesh by weight more than 80% using milling apparatus first, obtains a kind of high titanium slag powder, thenB, alkali leaching is miscellaneousHigh titanium slag powder that step A is obtained and concentration by weight 20 ~ 40% aqueous slkali according to solid-to-liquid ratio 1:5 ~ 8 is well mixed, It is placed in water-bath and carries out miscellaneous 60 ~ 120 min of alkali leaching at boiling temperature；Then filtered, washed and dried, obtain alkali The miscellaneous slag of leaching, thenC, modified roastingCarried out sodium carbonate is added in the miscellaneous slag of alkali leaching that step B is obtained as modifying agent, modified dosage is the miscellaneous slag weight of alkali leaching The 20 ~ 40% of amount, modifying agent is well mixed with the miscellaneous slag of alkali leaching, is carried out in microwave device under conditions of 700 ~ 900 DEG C micro- Wavefront modifier is calcined, and obtains a kind of modified titanium-rich slag, thenD, acidleach cleansModified titanium-rich slag that step C is obtained and concentration by weight 20 ~ 30% inorganic acid with solid-to-liquid ratio 1:4 ~ 6 is well mixed, It is placed in water-bath and carries out 60 ~ 120 min of acidleach removal of impurities at boiling temperatureThen filtered, washed and dried, obtain acidleach removal of impurities slag, thenE, calcineAcidleach that step D is obtained removal of impurities slag is put into crucible, is placed in microwave device in the temperature strip of 900 ~ 1000 DEG C of temperature Calcined under part, obtain the synthetic rutile.
- 2. according to the method described in claims 1, it is characterised in that in step A, the high titanium slag is TiO by weight2Content For more than 85.0%, SiO2For less than 4.0% titanium slag.
- 3. according to the method described in claims 1, it is characterised in that in step B, the aqueous slkali is sodium hydroxide solution.
- 4. according to the method described in claims 1, it is characterised in that in step C, the modification of sodium carbonate agent sodium sulphate or Phosphate replaces.
- 5. according to the method described in claims 1, it is characterised in that in step C, the microwave irradiation time is 30 ~ 60 min。
- 6. according to the method described in claims 1, it is characterised in that in step C, the frequency of the microwave device for 2350 ~ 2450MHz。
- 7. according to the method described in claims 1, it is characterised in that in step C, microwave is controlled during the microwave calcining Heating ramp rate is in 10 ~ 100/min.
- 8. according to the method described in claims 1, it is characterised in that in step D, the inorganic acid is sulfuric acid or hydrochloric acid.
- 9. according to the method described in claims 1, it is characterised in that in step E, the calcining is in frequency in microwave device 20 ~ 40 min are handled under conditions of 2350 ~ 2450MHz of rate.
- 10. according to the method described in claims 1, it is characterised in that the purity of the rutile is by weight more than 91%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109012566B (en) * | 2018-09-18 | 2021-08-06 | 渤海大学 | Preparation method of material for removing organic pollutants in hypochlorous white mud based petroleum wastewater |
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