CN106241864A - Acidolysis pot and the acid hydrolysis method of titaniferous material - Google Patents
Acidolysis pot and the acid hydrolysis method of titaniferous material Download PDFInfo
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- CN106241864A CN106241864A CN201610575904.6A CN201610575904A CN106241864A CN 106241864 A CN106241864 A CN 106241864A CN 201610575904 A CN201610575904 A CN 201610575904A CN 106241864 A CN106241864 A CN 106241864A
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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
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
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Abstract
The invention discloses a kind of acidolysis pot, including inverted cone portion, the bottom in inverted cone portion is provided with compressed air distribution grid, and the sidewall in inverted cone portion is circumferentially evenly arranged multiple compressed air hose stretching into pot nside;What compressed air hose exported is shaped as horn mouth, and bell-mouthed big opening end is positioned at the inner side of sidewall, bell-mouthed vertex angle theta >=45 °.The invention also discloses the acid hydrolysis method of a kind of titaniferous material, use above-mentioned acidolysis pot to carry out, comprise the following steps: the acidolysis premix of sulphuric acid with titaniferous material is added acidolysis pot;By compressed air hose with 200~400m3The flow of/h is passed through compressed air in acidolysis pot;At the end for the treatment of acidolysis primary response, stop in acidolysis pot, be passed through compressed air, carry out ripening;After ripening terminates, by compressed air hose with 50~100m3The flow of/h is passed through compressed air in acidolysis pot until acidolysis reaction terminates.Can effectively reduce the solid formation remaining in acidolysis pot.
Description
Technical field
The invention belongs to sulfate process titanium dioxide preparation field, particularly relate to a kind of device and method reducing acidolysis solid formation.
Background technology
Using in Titanium White Production By Sulfuric Acid Process technique, the hydrolysis procedure overwhelming majority is for using clearance-type to produce, and it fills
Standby predominantly acidolysis pot, traditional acidolysis pot, the only bottom at acidolysis pot are provided with compressed air distribution grid, in acid hemolysis process,
In pot, it is passed through compressed air by compressed air distribution grid to be stirred.When change occur in titanium material, public auxiliary condition, such as figure
Shown in 1, often pile up acidolysis residual solid phase in the tapered portion of acidolysis pot and the binding site of tapered portion and intermediate cylinder body
Thing, i.e. has not dissolved in the solid aggregates of water.
It is deposited in the tapered portion of acidolysis pot and the acidolysis residual solid phase thing of the binding site of tapered portion and intermediate cylinder body
Production be will result in large effect, be mainly reflected in three aspects: 1. directly influence the yield of acid hemolysis process titanium;The most serious
Affecting production yields, increasing of acidolysis residual solid phase thing causes acidolysis pot dischargeable capacity to reduce, and single batch acidolysis inventory reduces;
3. have a strong impact on production safety, owing to acidolysis residual solid phase thing remains essentially in the bottom of acidolysis pot, affect in acid hemolysis process and press
Space division cloth, is easily caused acidolysis and emits pot.Therefore, it is urgently to be resolved hurrily in titanium powder industry that acidolysis residual solid phase thing is decreased or even eliminated
Technical problem.
In order to eliminate the acidolysis solid formation of generation, the method generally used is saucepan, i.e. to acidolysis pot after blowing terminates
The appropriate spent acid of middle addition, is passed through steam heated and boiled from bottom.Boil once pot and generally to consume several days time, and solid formation is removed
Effect is not ideal enough, and in the slurry produced after saucepan, titanium dioxide cannot recycle, causes the loss of titanium.
The method is the processing method of a kind of " passively ", and in acid hemolysis process, how being decreased or even eliminated of " actively "
Solid formation will be the direction of emphasis consideration.In terms of the minimizing solid formation of " actively ", numerous studies, typically literary composition in industry, are done
Offer as follows:
Chinese invention patent " a kind of acidolysis premixing system reducing breeze and concentrated sulphuric acid formation solid formation " is by optimizing acid
Solve premix change system and reduce solid formation.
" sulfate process titanium dioxide eliminates acidolysis in producing to the paper of Sichuan non-ferrous metal (phase calendar year 2001 the 4th) author He Mingchuan etc.
Residual solid phase thing improves the approach of acidolysis rate " cut down acidolysis by the angle of compressed air distribution plate orifices bottom change acidolysis pot
Solid formation.
The paper " premixing process impact on titanium ore acidolysis " of steel vanadium titanium (the 6th phase in 2013) author Wu Jianchun etc. is mentioned
Avoid too much producing acidolysis solid formation by optimizing premixing process.
The method that document above is mentioned has certain help to reducing acidolysis solid formation, but effect is very limited, particularly
When there is large change in titanium ore mineral resources or public auxiliary condition.
Summary of the invention
First technical problem to be solved by this invention is to provide a kind of taper that can effectively reduce and remain in acidolysis pot
The acidolysis pot of the solid formation of the binding site of portion and tapered portion and intermediate cylinder body.
The present invention solves the acidolysis pot that first technical problem is used, including inverted cone portion, the end in described inverted cone portion
Portion is provided with compressed air distribution grid, and the sidewall in described inverted cone portion is circumferentially evenly arranged multiple pot nside that stretches into
Compressed air hose;What described compressed air hose exported is shaped as horn mouth, and described bell-mouthed big opening end is positioned at the inner side of sidewall,
Described bell-mouthed vertex angle theta >=45 °.
Preferably, described 80 °≤θ≤120 ° of bell-mouthed drift angle.
Preferably, quantity >=4 of described compressed air hose.
Preferably, the 60 °≤Φ of angle between the centrage in described bell-mouthed centrage and described inverted cone portion≤
90°。
Preferably, distance H between center and the top in inverted cone portion of described bell-mouthed big opening end is inverted cone portion
Height 1/3~1/2.
Preferably, the distance≤20cm between center and the sidewall in inverted cone portion of described bell-mouthed big opening end.
Second technical problem to be solved by this invention is to provide a kind of taper that can effectively reduce and remain in acidolysis pot
The acid hydrolysis method of the titaniferous material of the solid formation of the binding site of portion and tapered portion and intermediate cylinder body.
The present invention solves the acid hydrolysis method of the titaniferous material that second technical problem is used, and uses above-mentioned acidolysis pot to enter
OK, comprise the following steps:
A, the acidolysis premix of sulphuric acid and titaniferous material is added acidolysis pot;
B, by compressed air hose with 200~400m3The flow of/h is passed through compressed air in acidolysis pot;
C, treat acidolysis primary response at the end of, stop in acidolysis pot, be passed through compressed air, carry out ripening;
D, after ripening terminates, by compressed air hose with 50~100m3The flow of/h is passed through compression sky in acidolysis pot
Gas is until acidolysis reaction terminates.
Preferably, in step A, sulphuric acid is 1.5~1.75:1 with the mass ratio of titaniferous material.
Preferably, in step A, described titaniferous material is ilmenite, and sulphuric acid is 1.5~1.55 with the mass ratio of ilmenite:
1。
Preferably, in step A, described titaniferous material is titanium slag, and sulphuric acid is 1.7~1.75:1 with the mass ratio of titanium slag.
The invention has the beneficial effects as follows: when using the acidolysis pot of the present invention that titaniferous material is carried out acidolysis, not only from back taper
Compressed air distribution grid bottom shape portion is passed through compressed air in acidolysis pot and is stirred, and from the sidewall in inverted cone portion
The multiple compressed air hoses stretching into pot nside being circumferentially evenly arranged are passed through compressed air in acidolysis pot and are stirred, pressure
Contracting air pipe outlets be shaped as horn mouth, bell-mouthed big opening end is positioned at the inner side of sidewall, and bell-mouthed vertex angle theta >=45 °,
And in acid hemolysis process, by by the flow-control of compressed air hose in particular range, acidolysis pot can be effectively improved intrinsic pressure
The airflow field distribution of contracting air, the position making existing acidolysis pot there is airflow field dead angle has good mixing effect, it is ensured that
During acidolysis primary response, the uniformity of stirring, makes acidolysis reaction product porous, and leaching is easier to, thus reduces and even eliminate
Remain in the tapered portion of acidolysis pot and the solid formation of the binding site of tapered portion and intermediate cylinder body, when bell-mouthed drift angle is
80 °≤θ≤120 °, using the acidolysis pot of the present invention that titaniferous material is carried out acidolysis, it reduces the tapered portion remaining in acidolysis pot
And tapered portion is best with the effect of the solid formation of the binding site of intermediate cylinder body.
Accompanying drawing explanation
Fig. 1 is the structural representation of prior art;
Fig. 2 is the structural representation of the present invention;
Fig. 3 is the enlarged diagram of compressed air hose;
Shown in figure: inverted cone portion 1, sidewall 11, compressed air hose 2, big opening end 21, valve 3, compressed air are divided
Fabric swatch 4, intermediate cylinder body 5, acidolysis residual solid phase thing 6.
Detailed description of the invention
The present invention is further described with embodiment below in conjunction with the accompanying drawings.
As shown in Figures 2 and 3, the acidolysis pot of the present invention, including inverted cone portion 1, the bottom in described inverted cone portion 1 is provided with
Compressed air distribution grid 4, the sidewall 11 in described inverted cone portion 1 is circumferentially evenly arranged multiple compression stretching into pot nside
Air hose 2;What described compressed air hose 2 exported is shaped as horn mouth, and described bell-mouthed big opening end 21 is positioned at sidewall 11
Side, described bell-mouthed vertex angle theta >=45 °.
Wherein, inverted cone portion 1 refers to the bore bullet more than the bore of bottom at top;On compressed air hose 2 close
The position of acidolysis pot is provided with valve 3, in order to operator control whether to be passed through compression sky by switch or closedown valve 3
Gas, controls compressed-air actuated uninterrupted by the unlatching size of control valve 3, and certainly, valve 3 can also be arranged on compression
The entrance point of air hose 2, on the compressed-air actuated equipment of manufacture that valve 3 can also be arranged on compressed air hose 2 is connected.
When the acidolysis pot using the present invention carries out acidolysis, not only the compressed air distribution grid 4 bottom inverted cone portion 1 is to acid
It is passed through compressed air in solving pot to be stirred, and is circumferentially evenly arranged many from the sidewall 11 being arranged on inverted cone portion 1
The individual compressed air hose 2 stretching into pot nside is passed through compressed air in acidolysis pot and is stirred, the shape of compressed air hose 2 outlet
Shape is horn mouth, and bell-mouthed big opening end 21 is positioned at the inner side of sidewall 11, and bell-mouthed vertex angle theta >=45 °, can be effectively improved
The airflow field distribution of acidolysis pot compressed air, the position making existing acidolysis pot there is airflow field dead angle has good stirring
Effect, it is ensured that the uniformity of stirring during acidolysis primary response, makes acidolysis reaction product porous, and leaching is easier to, thus subtracts
Little even elimination remains in the tapered portion of acidolysis pot and the solid formation of the binding site of tapered portion and intermediate cylinder body.
Bell-mouthed vertex angle theta is the least, and the compressed air of adjacent sidewalls is concentrated very much, and bell-mouthed vertex angle theta is too big, adjacent sidewalls
Compressed air disperse very much, be all unfavorable for the uniformity of stirring, it is preferred, therefore, that described 80 °≤θ of bell-mouthed drift angle≤
120°。
The quantity of compressed air hose 2 can be odd number, it is also possible to is even number, as long as ensureing to be evenly distributed on inverted cone
In the circumference of the sidewall 11 in portion 1, quantity is the most, so that stirring is evenly, it is preferred that described compressed air hose 2
Quantity >=4, further preferably, the quantity of described compressed air hose 2 is even number.
In order to improve the uniformity of stirring further, as preferred embodiment, described bell-mouthed centrage and institute
State 60 °≤Φ≤90 ° of angle between the centrage in inverted cone portion 1, namely when the pot of acidolysis pot is vertically placed on horizontal plane
Time upper, bell-mouthed opening direction is horizontal direction or oblique top, so that tapered portion and the combination of intermediate cylinder body
Position can effectively be stirred, and reduces the residual solid formation at this.
In order to improve the uniformity of stirring further, as preferred embodiment, described bell-mouthed big opening end 21
Distance H between the top in center and inverted cone portion 1 is the 1/2~1/3 of the height in inverted cone portion 1.
In order to improve the uniformity of stirring further, as preferred embodiment, described bell-mouthed big opening end 21 with
Distance≤20cm between the sidewall 11 in inverted cone portion 1.
The acid hydrolysis method of the titaniferous material of the present invention, uses the acidolysis pot of the present invention to carry out, comprises the following steps:
A, the acidolysis premix of sulphuric acid and titaniferous material is added acidolysis pot;
B, by compressed air hose 2 with 200~400m3The flow of/h is passed through compressed air in acidolysis pot;
C, treat acidolysis primary response at the end of, stop in acidolysis pot, be passed through compressed air, carry out ripening;
D, after ripening terminates, by compressed air hose 2 with 50~100m3The flow of/h is passed through compression sky in acidolysis pot
Gas is until acidolysis reaction terminates.
Wherein, the acidolysis pot that the using method of the compressed air distribution grid 4 of the bottom in inverted cone portion 1 is traditional with this area
Using method is identical, does not repeats them here.
Wherein, sulphuric acid generally uses the concentrated sulphuric acid of 96%~98%, and titaniferous material can be the raw material containing titanium oxide,
Titaniferous material commonly used in the art is all applicable to the present invention, such as: at least one in ilmenite, titanium slag;Commonly used in the art
Titaniferous material is all applicable to the present invention with the mass ratio of sulphuric acid, it is preferred that in step A, sulphuric acid with the mass ratio of titaniferous material is
1.5~1.75:1.
Described titaniferous material is relevant with the kind of titaniferous material to the mass ratio of sulphuric acid, it is preferable that described titaniferous material is titanium
Iron mine, sulphuric acid is 1.5~1.55:1 with the mass ratio of ilmenite;Preferably, described titaniferous material is titanium slag, sulphuric acid and the matter of titanium slag
Amount ratio is 1.7~1.75:1.
Embodiment 1:
4 compressed air hoses stretching into pot nside circumferentially it are evenly arranged on the sidewall in the inverted cone portion of acidolysis pot,
Bell-mouthed vertex angle theta is 90 °, and the angle Φ between the centrage in bell-mouthed centrage and inverted cone portion is 90 °, bell-mouthed
1/2 of the height that distance H is inverted cone portion between center and the top in inverted cone portion of big opening end, bell-mouthed big opening end
Distance between the sidewall in center and inverted cone portion is 10cm;Acidolysis premixing by sulphuric acid that mass ratio is 1.52 with ilmenite
Thing adds acidolysis pot;By compressed air hose 2 with 300m3The flow of/h is passed through compressed air in acidolysis pot;Treat that acidolysis master is anti-
At the end of Ying, stop in acidolysis pot, be passed through compressed air, carry out ripening;After ripening terminates, by compressed air hose 2 with
70m3The flow of/h is passed through compressed air in acidolysis pot until acidolysis reaction terminates.After reaction terminates, solid in observation acidolysis pot
Phase thing, about 1m3。
Comparative example 1:
Use traditional acidolysis pot to carry out acidolysis, the acidolysis premix of sulphuric acid that mass ratio is 1.52 with ilmenite is added
Enter acidolysis pot and carry out acidolysis reaction.After reaction terminates, solid formation, about 5m in observation acidolysis pot3。
Embodiment 2:
6 compressed air hoses stretching into pot nside circumferentially it are evenly arranged on the sidewall in the inverted cone portion of acidolysis pot,
Bell-mouthed vertex angle theta is 100 °, and the angle Φ between the centrage in bell-mouthed centrage and inverted cone portion is 80 °, horn mouth
Big opening end center and the top in inverted cone portion between the height that distance H is inverted cone portion 1/3, bell-mouthed big opening end
Center and the sidewall in inverted cone portion between distance be 15cm;Acidolysis premixing by sulphuric acid that mass ratio is 1.72 with titanium slag
Thing adds acidolysis pot;By compressed air hose 2 with 250m3The flow of/h is passed through compressed air in acidolysis pot;Treat that acidolysis master is anti-
At the end of Ying, stop in acidolysis pot, be passed through compressed air, carry out ripening;After ripening terminates, by compressed air hose 2 with
60m3The flow of/h is passed through compressed air in acidolysis pot until acidolysis reaction terminates.After reaction terminates, solid in observation acidolysis pot
Phase thing, about 1.5m3。
Comparative example 2:
Use traditional acidolysis pot to carry out acidolysis, the acidolysis premix of sulphuric acid that mass ratio is 1.72 with titanium slag is added
Acidolysis pot carries out acidolysis reaction.After reaction terminates, solid formation, about 6m in observation acidolysis pot3。
Embodiment 3:
6 compressed air hoses stretching into pot nside circumferentially it are evenly arranged on the sidewall in the inverted cone portion of acidolysis pot,
Bell-mouthed vertex angle theta is 80 °, and the angle Φ between the centrage in bell-mouthed centrage and inverted cone portion is 70 °, bell-mouthed
1/3 of the height that distance H is inverted cone portion between center and the top in inverted cone portion of big opening end, bell-mouthed big opening end
Distance between the sidewall in center and inverted cone portion is 5cm;Acidolysis premix by sulphuric acid that mass ratio is 1.75 with titanium slag
Add acidolysis pot;By compressed air hose 2 with 350m3The flow of/h is passed through compressed air in acidolysis pot;Treat acidolysis primary response
At the end of, stop in acidolysis pot, be passed through compressed air, carry out ripening;After ripening terminates, by compressed air hose 2 with
90m3The flow of/h is passed through compressed air in acidolysis pot until acidolysis reaction terminates.After reaction terminates, solid in observation acidolysis pot
Phase thing, about 0.8m3。
Comparative example 3:
Use traditional acidolysis pot to carry out acidolysis, the acidolysis premix of sulphuric acid that mass ratio is 1.7 with titanium slag is added
Acidolysis pot carries out acidolysis reaction.After reaction terminates, solid formation, about 5.0m in observation acidolysis pot3。
Embodiment 4:
6 compressed air hoses stretching into pot nside circumferentially it are evenly arranged on the sidewall in the inverted cone portion of acidolysis pot,
Bell-mouthed vertex angle theta is 120 °, and the angle Φ between the centrage in bell-mouthed centrage and inverted cone portion is 90 °, horn mouth
Big opening end center and the top in inverted cone portion between the height that distance H is inverted cone portion 5/12, bell-mouthed big mouth
Distance between center and the sidewall in inverted cone portion of end is 20cm;By pre-with the acidolysis of ilmenite for sulphuric acid that mass ratio is 1.54
Mixture adds acidolysis pot;By compressed air hose 2 with 400m3The flow of/h is passed through compressed air in acidolysis pot;Treat acidolysis
At the end of primary response, stop in acidolysis pot, be passed through compressed air, carry out ripening;After ripening terminates, by compressed air hose 2
With 100m3The flow of/h is passed through compressed air in acidolysis pot until acidolysis reaction terminates.After reaction terminates, in observation acidolysis pot
Solid formation, about 1.0m3。
Comparative example 4:
Use traditional acidolysis pot to carry out acidolysis, the acidolysis premix of sulphuric acid that mass ratio is 1.54 with ilmenite is added
Enter acidolysis pot and carry out acidolysis reaction.After reaction terminates, solid formation, about 4.5m in observation acidolysis pot3。
Embodiment 5:
4 compressed air hoses stretching into pot nside circumferentially it are evenly arranged on the sidewall in the inverted cone portion of acidolysis pot,
Bell-mouthed vertex angle theta is 60 °, and the angle Φ between the centrage in bell-mouthed centrage and inverted cone portion is 90 °, bell-mouthed
1/2 of the height that distance H is inverted cone portion between center and the top in inverted cone portion of big opening end, bell-mouthed big opening end
Distance between the sidewall in center and inverted cone portion is 10cm;Acidolysis premixing by sulphuric acid that mass ratio is 1.52 with ilmenite
Thing adds acidolysis pot;By compressed air hose 2 with 300m3The flow of/h is passed through compressed air in acidolysis pot;Treat that acidolysis master is anti-
At the end of Ying, stop in acidolysis pot, be passed through compressed air, carry out ripening;After ripening terminates, by compressed air hose 2 with
70m3The flow of/h is passed through compressed air in acidolysis pot until acidolysis reaction terminates.After reaction terminates, solid in observation acidolysis pot
Phase thing, about 2m3。
Embodiment 6:
6 compressed air hoses stretching into pot nside circumferentially it are evenly arranged on the sidewall in the inverted cone portion of acidolysis pot,
Bell-mouthed vertex angle theta is 135 °, and the angle Φ between the centrage in bell-mouthed centrage and inverted cone portion is 90 °, horn mouth
Big opening end center and the top in inverted cone portion between the height that distance H is inverted cone portion 5/12, bell-mouthed big mouth
Distance between center and the sidewall in inverted cone portion of end is 20cm;By pre-with the acidolysis of ilmenite for sulphuric acid that mass ratio is 1.54
Mixture adds acidolysis pot;By compressed air hose 2 with 400m3The flow of/h is passed through compressed air in acidolysis pot;Treat acidolysis
At the end of primary response, stop in acidolysis pot, be passed through compressed air, carry out ripening;After ripening terminates, by compressed air hose 2
With 100m3The flow of/h is passed through compressed air in acidolysis pot until acidolysis reaction terminates.After reaction terminates, in observation acidolysis pot
Solid formation, about 1.7m3。
Claims (10)
1. acidolysis pot, including inverted cone portion (1), the bottom of described inverted cone portion (1) is provided with compressed air distribution grid (4), its
It is characterised by: on the sidewall (11) of described inverted cone portion (1), be circumferentially evenly arranged multiple compression sky stretching into pot nside
Trachea (2);What described compressed air hose (2) exported is shaped as horn mouth, and described bell-mouthed big opening end (21) is positioned at sidewall
(11) inner side, described bell-mouthed vertex angle theta >=45 °.
2. acidolysis pot as claimed in claim 1, it is characterised in that: described bell-mouthed 80 °≤θ≤120 ° of drift angle.
3. acidolysis pot as claimed in claim 1 or 2, it is characterised in that: quantity >=4 of described compressed air hose (2).
4. acidolysis pot as claimed any one in claims 1 to 3, it is characterised in that: described bell-mouthed centrage is with described
60 °≤Φ≤90 ° of angle between the centrage in inverted cone portion (1).
5. the acidolysis pot as according to any one of Claims 1-4, it is characterised in that: described bell-mouthed big opening end (21)
Distance H between the top of center and inverted cone portion (1) is the 1/3~1/2 of the height in inverted cone portion (1).
6. the acidolysis pot as according to any one of claim 1 to 5, it is characterised in that: described bell-mouthed big opening end (21)
Distance≤20cm between the sidewall (11) of center and inverted cone portion (1).
7. the acid hydrolysis method of titaniferous material, is characterised by: use the acidolysis pot as according to any one of claim 1 to 6 to carry out,
Comprise the following steps:
A, the acidolysis premix of sulphuric acid and titaniferous material is added acidolysis pot;
B, by compressed air hose (2) with 200~400m3The flow of/h is passed through compressed air in acidolysis pot;
C, treat acidolysis primary response at the end of, stop in acidolysis pot, be passed through compressed air, carry out ripening;
D, after ripening terminates, by compressed air hose (2) with 50~100m3The flow of/h is passed through compressed air in acidolysis pot
Until acidolysis reaction terminates.
8. the acid hydrolysis method of titaniferous material as claimed in claim 7, is characterised by: in step A, sulphuric acid and the matter of titaniferous material
Amount ratio is 1.5~1.75:1.
9. the acid hydrolysis method of titaniferous material as claimed in claim 8, is characterised by: in step A, and described titaniferous material is ferrotianium
Ore deposit, sulphuric acid is 1.5~1.55:1 with the mass ratio of ilmenite.
10. the acid hydrolysis method of titaniferous material as claimed in claim 8, is characterised by: in step A, and described titaniferous material is titanium
Slag, sulphuric acid is 1.7~1.75:1 with the mass ratio of titanium slag.
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CN114988465A (en) * | 2022-04-22 | 2022-09-02 | 甘肃东方钛业有限公司 | Efficient recycling method for scale in acidolysis premixing tank |
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