CN107720809A - A kind of mechanical activation combines the method for preparing synthetic rutile with microwave calcination - Google Patents
A kind of mechanical activation combines the method for preparing synthetic rutile with microwave calcination Download PDFInfo
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- CN107720809A CN107720809A CN201610650908.6A CN201610650908A CN107720809A CN 107720809 A CN107720809 A CN 107720809A CN 201610650908 A CN201610650908 A CN 201610650908A CN 107720809 A CN107720809 A CN 107720809A
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- C01G23/00—Compounds of titanium
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- C01G23/047—Titanium dioxide
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Abstract
The present invention relates to a kind of mechanical activation to combine the method for preparing synthetic rutile with microwave heating, and this method includes the step such as mechanical activation, microwave heating.The present invention is pre-processed by the way of mechanical activation to high titanium slag, can efficiently separate the Ti in the ilmenite component of high titanium slag2O3, the high temperature preprocessing process of alternative high titanium slag;In addition, the present invention, by the way of microwave heating, energy consumption is low, pollution-free, efficiency high, and clean manufacturing can be achieved.The adaptability to raw material of this method is strong, and can be made TiO2 contents by weight more than 92% synthetic rutile.
Description
Technical field
The present invention relates to a kind of preparation method of synthetic rutile, specifically it is a kind of by high titanium slag by mechanical activation,
The method that microwave treatment prepares synthetic rutile.
Background technology
It is added to a certain amount of carbon containing reducer of ilmenite supplying in electric furnace and carries out reduction melting, the oxygen of iron in ilmenite
Compound is selectively reduced to metallic iron, and titanyl compound to form titanium slag by being enriched with.High titanium slag is a kind of ilmenite concentrate
Or enrichment titanium ore.The grade for the rich-titanium material TiO2 that traditional electro-smelting ilmenite prepares in 60%-70% by weight,
Content of calcium and magnesium is up to 4% ~ 7%.But chloridising production titanium white requires the TiO in raw material2Content be more than 90%, and CaO+MgO is small
In 1.5%.
CN200810177520 discloses a kind of preparation method of synthetic rutile, and ilmenite concentrate is carried out into oxidizing roasting and gone back
Original roasting, removes the impurity in the product of reduction roasting, the product after removing impurity is calcined, oxidizing roasting is in oxidizing gas
Lower progress, reduction roasting are carried out under reducibility gas, and oxidation, reduction roasting are carried out in a fluidized bed reactor.The technique stream
Stateization requires higher with high-tension apparatus.CN20120280443 discloses a kind of method that synthetic rutile is prepared with titanium slag, first
Titanium slag is subjected to oxidizing roasting in 800 DEG C ~ 1000 DEG C, then reduction roasting is carried out in 700 DEG C ~ 900 DEG C, obtains being modified titanium slag;
Then one section of normal pressure or normal pressure multistage counter current Fluidizing Leaching are carried out to modified titanium slag using the initial leachate of watery hydrochloric acid;Leach
Cheng Houzai carries out countercurrent washing, and the technological process is complicated, and operation difficulty is big, is unfavorable for putting into industrial production.
In order to solve technological deficiency existing for prior art, the present inventor is on the basis of existing experiment is summarized, by big
Experimental study and analysis are measured, completes the present invention finally.
The content of the invention
Technical problem
It is an object of the invention to provide a kind of preparation method of synthetic rutile.This method is heated using microwave irradiation, equipment letter
Single, energy consumption is low, and accessory substance is less, meets energy-saving and emission-reduction and the requirement of clean energy.
Technical scheme]
The present invention is achieved through the following technical solutions.
The present invention designs a kind of preparation method of synthetic rutile.
The step of preparation method, is as follows:
A, mechanical activation
A certain amount of high titanium slag is put into drying box under conditions of 373K and dries 2h, is added in 400ml ball grinders, during ball milling
Between be 5-20h, obtain by the high titanium slag after mechanical activation.
B, microwave calcination
Microwave calcination is carried out under conditions of being 800 DEG C ~ 1100 DEG C in temperature by the high titanium slag that step A is obtained, obtains described people
Make rutile.
A preferred embodiment of the invention, in step, the high titanium slag are TiO by weight2Content is
More than 73%, SiO2It is less than 2.5% titanium slag for being less than 0.5% with CaO for less than 2.4%, MgO;The high titanium slag granularity is-
100 mesh are by weight more than 80%.
According to another preferred embodiment of the present invention, in step, ball-milling medium mass ratio is 1:15~1:1.
According to another preferred embodiment of the present invention, in step, rotational speed of ball-mill is set as 200 ~ 450rpm.
According to another preferred embodiment of the present invention, in stepb, the power of described microwave reactor is
3.0kw~6.0kw。
According to another preferred embodiment of the present invention, in stepb, the frequency of the microwave reactor for 912 ~
920MHZ。
According to another preferred embodiment of the present invention, in stepb, the frequency of the microwave reactor for 912 ~
918MHZ。
According to the present invention another preferred embodiment, in stepb, in the tangible microwave reactor of described calcining
Frequency handles 1h ~ 2h under conditions of being 912 ~ 918MHZ.
According to another preferred embodiment of the present invention, in step C, the purity of the synthetic rutile is with weight
Meter more than 92%.
The present invention is described in more detail below
The present invention relates to a kind of preparation method of synthetic rutile.
The present invention uses mechanical activation and microwave irradiation Combined Treatment high titanium slag.First, mechanical activation can cause at a low price
State component is separated from the ilmenite composition of high titanium slag.Second, microwave irradiation processing can make valuable mineral and gangue solution
From, increase the effective affecting acreage of valuable mineral, promote interfacial chemical reaction, third, microwave heating treatment energy consumption is low, accessory substance
It is few, meet energy-saving and emission-reduction and the requirement of clean energy.
The preparation method is as follows:
A, mechanical activation c
A certain amount of high titanium slag is put into drying box under conditions of 373K and dries 120min, is added in 400ml ball grinders, ball
Consume time as 5-20h, obtain by the high titanium slag after mechanical activation.
The high titanium slag that the present invention uses is the titanium slag obtained by removing after most of iron by electro-smelting.The present invention makes
High titanium slag typically has following chemical compositions:TiO by weight2Content is more than 73%, SiO2It is for less than 2.4%, MgO
Less than 2.5% with CaO be less than 0.5% titanium slag;The high titanium slag granularity is -100 mesh for by weight more than 80%.
Wherein TiO2It is to be determined according to GB/T1706-2006 standards using aluminum reduction method.Al2O3It is according to GB15892-
2009 standards are using EDTA complexing villiaumite titration measurings.Iron and ferriferous oxide are used according to YB/T505.5-2007 standards
Spectrophotometry.SiO2It is to be determined according to YB/T190.1-2001 standards using perchloric acid determination.MgO is
According to YB/T 190.4-2001 standards using CyDTA titration measurings.CaO is used according to YSBC19811-2000 standards
Aas determination.
The granularity of the high titanium slag is -100 mesh for by weight more than 80%.If the granularity of the high titanium slag is not met
It is required, existing pulverising apparatus can be used to carry out pulverization process with screening plant, such as by the great prosperous mining machinery in Shicheng County
Manufactory is with trade name sealed type sample pulverizer(MZ-200)The pulverising apparatus of sale, Shanghai Yichang instrument Sha Shai factories are by with business
The screening plant of name of an article standard screen sale.
The drying box that the present invention uses is current market sales of product, such as instrument and meter Co., Ltd is established in Shanghai
The drying box sold with trade name electric drying oven with forced convection (FX101-1 types)
The ball mill that the present invention uses is current market sales of product, such as has Nanjing Nanda Instrument Co., Ltd. with commodity
The ball mill of name planetary ball mill (QM-3SP4 types) sale.
In the present invention, mechanical activation is it should be understood that a kind of processing for changing high titanium slag thing phase composition, the purpose is to will
Lower valency titanium component in ilmenite is separated.
In the present invention, if ball-milling medium mass ratio is less than 1:1, then it can activate not exclusively, still there is part high titanium slag
Ti2O3Component fails to separate;If ball-milling medium mass ratio is more than 1:15, then separating effect do not have more significant change;
Therefore, ball-milling medium mass ratio is 1:15~1:1 be it is rational, preferably 1:12~1:4.
In the present invention, if the mechanical activation time is less than 5h, it can activate not exclusively, if greater than 20h, then can produce
Excessive and unnecessary energy consumption;Therefore, the processing time of this mechanical activation be 5h ~ 20h be it is appropriate, preferably 8h ~
17h, more preferably 10h ~ 15h.
B, mechanical activation
Microwave calcination is carried out under conditions of being 800 DEG C ~ 1100 DEG C in temperature by the high titanium slag that step A is obtained, obtains described people
Make rutile.
The microwave heating equipment that the present invention uses is current market sales of product, such as by long Thailand of salon microwave thermal technology
Co., Ltd is with trade name microwave Muffle furnace(HAMiLab-M/As types)The microwave Muffle furnace of sale.
The microwave irradiation treatment temperature is 800 DEG C ~ 1100 DEG C.If irradiation temperature is less than 800 DEG C, titanium dioxide is brilliant
Type transformation is insufficient, and part anatase titanium dioxide can not be converted into rutile-type;If irradiation temperature is higher than 1100 DEG C,
Occur sintering phenomenon, thus calcining heat be 800 DEG C ~ 1100 DEG C be it is feasible, preferably 850 DEG C ~ 1050 DEG C, more preferably
Ground is 900 DEG C ~ 1000 DEG C.
The microwave irradiation processing time is 1h ~ 2h.If microwave irradiation time is less than 1h, the reaction of titanium slag calcination for activation
Not enough fully, anosovite solid solution structure destroys not abundant enough, and Crystalline Phase Transition of Titania process is not abundant enough;If microwave spoke
It is more than 2h according to processing time, then reacts and be substantially saturated, continuing increases exposure time influences less on reaction result;Therefore, spoke
It is that 1h ~ 2h is rational, preferably 1.2h ~ 1.8h according to processing time, more preferably 1.3h ~ 1.5h.
Beneficial effect]
The beneficial effects of the invention are as follows:The present invention takes mechanical activation to handle so that Ti before high titanium slag calcining2O3From height
Separated in the ilmenite composition of titanium slag.The method can pre-process as a kind of new method instead of the high temperature of high titanium slag
Process.In addition, the present invention by the way of microwave heating, the characteristics of selectively heating to mineral using microwave, realizes titanium component
Selective enrichment, accelerate rutile TiO2Generating rate, and can be made TiO2 contents by weight more than 92% artificial gold
Red stone.
Embodiment
The present invention can be better understood from by following embodiments.
Embodiment 1:Microwave method prepares synthetic rutile
The embodiment implementation steps are as follows:
A, mechanical activation
Using by Shicheng County Hao Xin mining machineries manufactory with trade name sealed type sample pulverizer(MZ-200)The crushing of sale
The screening plant that equipment and Shanghai Yichang instrument Sha Shai factories are sold with trade name standard screen, granularity is crushed to weight by high titanium slag
Meter more than 80% is more than -100 mesh, obtains a kind of high titanium slag powder, then
A certain amount of high titanium slag is put into Shanghai and establishes instrument and meter Co., Ltd with trade name electric drying oven with forced convection (FX101-
1 type) under conditions of 373K dry 2h, add 400ml ball grinders in, Ball-milling Time 6h, obtain by after mechanical activation
High titanium slag.
B, microwave calcination
Using long microwave thermal technology Co., Ltd of Thailand of salon with trade name microwave Muffle furnace(HAMiLab-M/As types)The microwave of sale
Muffle furnace, TiO is obtained with being incubated 1.2h under conditions of 1000 DEG C of temperature in microwave power 4.0kw, frequency 912MHZ2Content with
The rutile of weight meter more than 92%.
Detected using assay method described in this description, rutile TiO manufactured in the present embodiment2Content be
92.06%th, S content is 0.014%, P content is 0.019% and C content is 0.023%, complies fully with chloridising production titanium
White requirement.
Embodiment 2:Microwave method prepares synthetic rutile
The embodiment implementation steps are as follows:
A, mechanical activation
Using by Shicheng County Hao Xin mining machineries manufactory with trade name sealed type sample pulverizer(MZ-200)The crushing of sale
The screening plant that equipment and Shanghai Yichang instrument Sha Shai factories are sold with trade name standard screen, granularity is crushed to weight by high titanium slag
Meter more than 80% is more than -100 mesh, obtains a kind of high titanium slag powder, then
A certain amount of high titanium slag is put into Shanghai and establishes instrument and meter Co., Ltd with trade name electric drying oven with forced convection (FX101-
1 type) under conditions of 373K dry 2h, add 400ml ball grinders in, Ball-milling Time 10h, obtain by after mechanical activation
High titanium slag.
B, microwave calcination
Using long microwave thermal technology Co., Ltd of Thailand of salon with trade name microwave Muffle furnace(HAMiLab-M/As types)The microwave of sale
Muffle furnace, TiO is obtained with being incubated 1.3h under conditions of 900 DEG C of temperature in microwave power 3.0kw, frequency 918MHZ2Content is with weight
The rutile of gauge more than 92%.
Detected using assay method described in this description, rutile TiO manufactured in the present embodiment2Content be
92.74%th, S content is 0.014%, P content is 0.03% and C content is 0.032%, complies fully with chloridising production titanium white
Requirement.
Embodiment 3:Microwave method prepares synthetic rutile
The embodiment implementation steps are as follows:
A, mechanical activation
Using by Shicheng County Hao Xin mining machineries manufactory with trade name sealed type sample pulverizer(MZ-200)The crushing of sale
The screening plant that equipment and Shanghai Yichang instrument Sha Shai factories are sold with trade name standard screen, granularity is crushed to weight by high titanium slag
Meter more than 80% is more than -100 mesh, obtains a kind of high titanium slag powder, then
A certain amount of high titanium slag is put into Shanghai and establishes instrument and meter Co., Ltd with trade name electric drying oven with forced convection (FX101-
1 type) under conditions of 373K dry 2h, add 400ml ball grinders in, Ball-milling Time 12h, obtain by after mechanical activation
High titanium slag.
B, microwave calcination
Using long microwave thermal technology Co., Ltd of Thailand of salon with trade name microwave Muffle furnace(HAMiLab-M/As types)The microwave of sale
Muffle furnace, TiO is obtained with being incubated 1.5h under conditions of 950 DEG C of temperature in microwave power 5.0kw, frequency 915MHZ2Content is with weight
The rutile of gauge more than 92%.
Detected using assay method described in this description, rutile TiO manufactured in the present embodiment2Content be
92.50%th, S content is 0.023%, P content is 0.02% and C content is 0.019%, complies fully with chloridising production titanium white
Requirement.
Embodiment 4:Microwave method prepares synthetic rutile
The embodiment implementation steps are as follows:
A, mechanical activation
Using by Shicheng County Hao Xin mining machineries manufactory with trade name sealed type sample pulverizer(MZ-200)The crushing of sale
The screening plant that equipment and Shanghai Yichang instrument Sha Shai factories are sold with trade name standard screen, granularity is crushed to weight by high titanium slag
Meter more than 80% is more than -100 mesh, obtains a kind of high titanium slag powder, then
A certain amount of high titanium slag is put into Shanghai and establishes instrument and meter Co., Ltd with trade name electric drying oven with forced convection (FX101-
1 type) under conditions of 373K dry 2h, add 400ml ball grinders in, Ball-milling Time 20h, obtain by after mechanical activation
High titanium slag.
B, microwave calcination
Using long microwave thermal technology Co., Ltd of Thailand of salon with trade name microwave Muffle furnace(HAMiLab-M/As types)The microwave of sale
Muffle furnace, TiO is obtained with being incubated 2h under conditions of 850 DEG C of temperature in microwave power 5.5kw, frequency 913MHZ2Content is with weight
The rutile of meter more than 92%.
Detected using assay method described in this description, rutile TiO manufactured in the present embodiment2Content be
92.06%th, S content is 0.017%, P content is 0.022% and C content is 0.019%, complies fully with chloridising production titanium
White requirement.
Embodiment 5:Microwave method prepares synthetic rutile
The embodiment implementation steps are as follows:
A, mechanical activation
Using by Shicheng County Hao Xin mining machineries manufactory with trade name sealed type sample pulverizer(MZ-200)The crushing of sale
The screening plant that equipment and Shanghai Yichang instrument Sha Shai factories are sold with trade name standard screen, granularity is crushed to weight by high titanium slag
Meter more than 80% is more than -100 mesh, obtains a kind of high titanium slag powder, then
A certain amount of high titanium slag is put into Shanghai and establishes instrument and meter Co., Ltd with trade name electric drying oven with forced convection (FX101-
1 type) under conditions of 373K dry 2h, add 400ml ball grinders in, Ball-milling Time 18h, obtain by after mechanical activation
High titanium slag.
B, microwave calcination
Using long microwave thermal technology Co., Ltd of Thailand of salon with trade name microwave Muffle furnace(HAMiLab-M/As types)The microwave of sale
Muffle furnace, TiO is obtained with being incubated 1.2h under conditions of 1100 DEG C of temperature in microwave power 4.0kw, frequency 916MHZ2Content with
The rutile of weight meter more than 92%.
Detected using assay method described in this description, rutile TiO manufactured in the present embodiment2Content be
92.16%th, S content is 0.017%, P content is 0.022% and C content is 0.019%, complies fully with chloridising production titanium
White requirement.
Comparative example 1:Prepare synthetic rutile
The implementation steps of the embodiment are as follows:
A, mechanical activation
Using by Shicheng County Hao Xin mining machineries manufactory with trade name sealed type sample pulverizer(MZ-200)The crushing of sale
The screening plant that equipment and Shanghai Yichang instrument Sha Shai factories are sold with trade name standard screen, granularity is crushed to weight by high titanium slag
Meter more than 80% is more than -100 mesh, obtains a kind of high titanium slag powder, then
A certain amount of high titanium slag is put into Shanghai and establishes instrument and meter Co., Ltd with trade name electric drying oven with forced convection (FX101-
1 type) under conditions of 373K dry 2h, add 400ml ball grinders in, Ball-milling Time 6h, obtain by after mechanical activation
High titanium slag.
B, calcine
Using 1.2h is incubated under conditions of 1000 DEG C of resistance furnace and temperature, TiO is obtained2Content by weight more than 92% golden red
Stone.
Detected using assay method described in this description, rutile TiO manufactured in the present embodiment2Content be
80.03%th, S content is 0.13%, P content is 0.18% and C content is 0.08%.
Comparative example 2:Prepare synthetic rutile
The implementation steps of the embodiment are as follows:
A, mechanical activation
Using by Shicheng County Hao Xin mining machineries manufactory with trade name sealed type sample pulverizer(MZ-200)The crushing of sale
The screening plant that equipment and Shanghai Yichang instrument Sha Shai factories are sold with trade name standard screen, granularity is crushed to weight by high titanium slag
Meter more than 80% is more than -100 mesh, obtains a kind of high titanium slag powder, then
A certain amount of high titanium slag is put into Shanghai and establishes instrument and meter Co., Ltd with trade name electric drying oven with forced convection (FX101-
1 type) under conditions of 373K dry 2h, add 400ml ball grinders in, Ball-milling Time 10h, obtain by after mechanical activation
High titanium slag.
B, calcine
Using 1.2h is incubated under conditions of 900 DEG C of resistance furnace and temperature, TiO is obtained2Content by weight more than 92% golden red
Stone.
Detected using assay method described in this description, rutile TiO manufactured in the present embodiment2Content be
77.26%th, S content is 0.19%, P content is 0.79% and C content is 0.80%.
Comparative example 3:Prepare synthetic rutile
The implementation steps of the embodiment are as follows:
A, mechanical activation
Using by Shicheng County Hao Xin mining machineries manufactory with trade name sealed type sample pulverizer(MZ-200)The crushing of sale
The screening plant that equipment and Shanghai Yichang instrument Sha Shai factories are sold with trade name standard screen, granularity is crushed to weight by high titanium slag
Meter more than 80% is more than -100 mesh, obtains a kind of high titanium slag powder, then
A certain amount of high titanium slag is put into Shanghai and establishes instrument and meter Co., Ltd with trade name electric drying oven with forced convection (FX101-
1 type) under conditions of 373K dry 2h, add 400ml ball grinders in, Ball-milling Time 12h, obtain by after mechanical activation
High titanium slag.
B, microwave calcination
1.5h is incubated under conditions of 950 DEG C of temperature using resistance furnace, obtains TiO2Content by weight more than 92% golden red
Stone.
Detected using assay method described in this description, rutile TiO manufactured in the present embodiment2Content be
76.62%th, S content is 0.19%, P content is 0.12% and C content is 0.72%.
Comparative example 4:Prepare synthetic rutile
The implementation steps of the embodiment are as follows:
A, mechanical activation
Using by Shicheng County Hao Xin mining machineries manufactory with trade name sealed type sample pulverizer(MZ-200)The crushing of sale
The screening plant that equipment and Shanghai Yichang instrument Sha Shai factories are sold with trade name standard screen, granularity is crushed to weight by high titanium slag
Meter more than 80% is more than -100 mesh, obtains a kind of high titanium slag powder, then
A certain amount of high titanium slag is put into Shanghai and establishes instrument and meter Co., Ltd with trade name electric drying oven with forced convection (FX101-
1 type) under conditions of 373K dry 2h, add 400ml ball grinders in, Ball-milling Time 20h, obtain by after mechanical activation
High titanium slag.
B, calcine
2h is incubated under conditions of 850 DEG C of temperature using long resistance furnace, obtains TiO2Content by weight more than 92% golden red
Stone.
Detected using assay method described in this description, rutile TiO manufactured in the present embodiment2Content be
75.72%th, S content is 0.23%, P content is 0.12% and C content is 0.76%.
Comparative example 5:Prepare synthetic rutile
The implementation steps of the embodiment are as follows:
A, mechanical activation
Using by Shicheng County Hao Xin mining machineries manufactory with trade name sealed type sample pulverizer(MZ-200)The crushing of sale
The screening plant that equipment and Shanghai Yichang instrument Sha Shai factories are sold with trade name standard screen, granularity is crushed to weight by high titanium slag
Meter more than 80% is more than -100 mesh, obtains a kind of high titanium slag powder, then
A certain amount of high titanium slag is put into Shanghai and establishes instrument and meter Co., Ltd with trade name electric drying oven with forced convection (FX101-
1 type) under conditions of 373K dry 2h, add 400ml ball grinders in, Ball-milling Time 18h, obtain by after mechanical activation
High titanium slag.
B, microwave calcination
1.2h is incubated under conditions of 1100 DEG C of temperature using resistance furnace, obtains TiO2Content by weight more than 92% golden red
Stone.
Detected using assay method described in this description, rutile TiO manufactured in the present embodiment2Content be
75.2%th, S content is 0.13%, P content is 0.18% and C content is 0.22%.
Example 1-5 result of implementation instructs with comparative example 1-5 result of implementation comparative analysis, using the inventive method
Obtain that synthetic rutile purity is higher than comparison example by 16.44%, this result be beyond expectations outside result.
Claims (8)
1. a kind of mechanical activation combines the method for preparing synthetic rutile with microwave heating, it is characterised in that the step of the preparation method
It is rapid as follows:
A, mechanical activation
A certain amount of high titanium slag is put into drying box under conditions of 373K and dries 2h, is added in 400ml ball grinders, during ball milling
Between be 5-20h, the high titanium slag after being activated, then;
B, microwave calcination
Microwave calcination is carried out under conditions of being 800 DEG C ~ 1100 DEG C in temperature by the high titanium slag that step A is obtained, obtains described people
Make rutile.
2. preparation method according to claim 1, it is characterised in that in step, the high titanium slag is TiO by weight2
Content is more than 73%, SiO2It is less than 2.5% titanium slag for being less than 0.5% with CaO for less than 2.4%, MgO;The high titanium slag grain
Degree is -100 mesh for by weight more than 80%.
3. preparation method according to claim 1, it is characterised in that in step, ball-milling medium mass ratio is 1:15~1:
1。
4. preparation method according to claim 1, it is characterised in that in step, set rotational speed of ball-mill as 200 ~
450rpm。
5. preparation method according to claim 1, it is characterised in that in stepb, the power of described microwave reactor
For 3.0kw ~ 6.0kw.
6. preparation method according to claim 1, it is characterised in that in stepb, the frequency of the microwave reactor is
912~918MHZ。
7. preparation method according to claim 1, it is characterised in that in stepb, the tangible microwave reaction of described calcining
In device 1h ~ 2h is handled under conditions of frequency is 912 ~ 918MHZ.
8. preparation method according to claim 1, it is characterised in that in step C, the purity of the synthetic rutile is
By weight more than 92%.
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CN107159402A (en) * | 2017-05-15 | 2017-09-15 | 东北大学 | A kind of technique of two-stage method mechanical activation boron concentrate |
CN107159402B (en) * | 2017-05-15 | 2019-02-05 | 东北大学 | A kind of technique of two-stage method mechanical activation boron concentrate |
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