CN109085153A - A kind of method for building up of the three-dimensional polar system of the titanium white washing Leaching Kinetics of characterization washing intensity - Google Patents
A kind of method for building up of the three-dimensional polar system of the titanium white washing Leaching Kinetics of characterization washing intensity Download PDFInfo
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- CN109085153A CN109085153A CN201810753996.1A CN201810753996A CN109085153A CN 109085153 A CN109085153 A CN 109085153A CN 201810753996 A CN201810753996 A CN 201810753996A CN 109085153 A CN109085153 A CN 109085153A
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Abstract
The invention discloses a kind of method for building up of the three-dimensional polar system of the titanium white washing Leaching Kinetics of characterization washing intensity, the present invention constructs the two-dimentional polar coordinate system for simplifying the vacuum filtration blade of dimensionality reduction first, binding time coordinate each event is with (t, r, θ) indicate, standard Special sample taker is reused for different event (t, r, θ) to sampling, weighing, drying, resolution, corresponding ion concentration is measured using flame atomic absorption spectrophotometer, further Concentration-time-area data is handled, integrate the data of different mineral resources, establish large database concept.By the above-mentioned means, the present invention compensates for a blank spot of current Producing Titanium Dioxide metatitanic acid washing process.Titanium sulfate plain boiled water can be optimized and wash process conditions, reduce sulfuric acid titanium powder industry washing process water, reduce expenses and the human costs such as technological operation power, shorten metatitanic acid and wash the production cycle.
Description
Technical field
The invention belongs to Titanium White Production By Sulfuric Acid Process technical fields, and in particular to a kind of titanium white washing of characterization washing intensity
The method for building up of the three-dimensional polar system of Leaching Kinetics.
Background technique
At present in the world, titanium dioxide (TiO2) production technology be mainly chloride process titanium dioxide and two kinds of sulfate process titanium dioxide.Sulphur
Acid system production titanium dioxide has had 90 years history, and because of its process route maturation, apparatus intensity requirement is low, to raw material
Grade requirement is low, while can produce the titanium dioxide of two kinds of crystal forms of rutile titania and rutile, and titanium white sulfuric acid process still has by force so far
Big vigor will complement each other, long-term co-existence with chloridising.And the important source material of production of titanium dioxide by sulfuric acid method is ilmenite
(FeTiO3), typically the content data based on X-ray fluorescence spectra is as shown in table 1 below for domestic common ilmenite.
The typical ilmenite X-ray fluorescence spectra data of table 1 (in terms of oxide)
Ilmenite is after acidolysis, purification, concentration, hydrolysis, the metatitanic acid (10H of generation2TiO3·SO3) adsorbed largely
The anion such as water-soluble metal heteroion and sulfate radical, the presence of these heteroions will affect calcine technology and last titanium
White powder quality, it is therefore necessary to these heteroions are removed before calcine technology.Titanium powder industry is using washed with impurities technique at present,
The washing workshop section can consume a large amount of process water, this is also the major reason that sulfuric acid titanium powder industry is referred to as highly water intensive industry.Absolutely
Most of producers washing equipment used in the workshop section is vacuum leaf filter, which is made of multiple groups filter plate, because
For the intrinsic vacuum of filter plate/suction filtration structure problem, the washing non-uniform phenomenon of filter cake is generally resulted in.Only in titration filtrate two
The experience of valence iron content and front-line workers far can not instruct and cope with the washing terminal of different situations hydrolyzation material.Often lead
It causes two aspect problems: first, washing intensity is insufficient, causing impurity content higher, influence final titanium dioxide quality.Second, washing
It is excessive to wash intensity, causes water consumption huger, while there are also the operating costs and human cost of vacuum pump.
Currently, domestic sulfate process titanium dioxide industry metatitanic acid washing workshop section is directed to leaf filter filter plate inherent structure, reply is different
Miberal powder and the liquid-solid extraction dynamics research of special unexpected hydrolysis situation are obviously insufficient, have not only lacked theory support but also without research hand
Section.And consumption of the problem concerning the production cycle, washing workshop section's power consumption, human cost especially wash water of titanium powder industry,
This is a blank spot of current titanium white enterprise metatitanic acid washing process.
Summary of the invention
The invention mainly solves the technical problem of providing a kind of titanium white washing Leaching Kinetics of characterization washing intensity
The method for building up of three-dimensional polar system compensates for a blank spot of current Producing Titanium Dioxide metatitanic acid washing process.
The technical solution adopted by the present invention is that: for the hydrolyzation material of different mineral and operating condition, use standard special-purpose taking
Semicontinuous acquisition event (t, r, the θ) sample of sample device, passes through flame atom spectrum measuring different time, spatial position sample
The miscellaneous tenor of point (t, r, θ), constructs and analyzes large database concept, establishes in standardized washing and controls system.
A kind of method for building up of the three-dimensional polar system of the titanium white washing Leaching Kinetics of characterization washing intensity, including with
Lower step:
(1) the two-dimentional polar coordinate system for simplifying the vacuum filtration blade of dimensionality reduction is constructed, each event is indicated with (t, r, θ), wherein t
The coordinate representation time；R coordinate representation is at a distance from pole；The angle of θ coordinate representation 0 ° of ray of coordinate distance counterclockwise；
(2) 0.1 is sampled to washing metatitanic acid filter disc for different events (t, r, θ) using standard Special sample taker ~
100g；
(3) it weighed, dried, 0.1 ~ 10h to above-mentioned sampling at a temperature of 0 ~ 120 DEG C；
(4) then using hydrochloric acid, sulfuric acid, nitric acid, perchloric acid, the one or more mixed acid of hydrobromic acid in 0 ~ 300 DEG C of temperature condition
Under 0.1 ~ 10h of resolution carried out to the sample dried in step (3), cooling, be settled to 10 ~ 1000ml；
(5) the miscellaneous concentration of metal ions that above-mentioned each constant volume solution is measured using flame atomic absorption spectrophotometer, calculates inclined titanium
Miscellaneous tenor in sour material；Typical processing formula is as follows, certain time point t1Corresponding heteroion concentration calculation formula is as follows:
Wherein:
S1, it is spatial point (t, r1, θ1) corresponding filter cake area；
S2, it is spatial point (t, r2, θ2) corresponding filter cake area；
S3, it is spatial point (t, r3, θ3) corresponding filter cake area；
S4, it is spatial point (t, r4, θ4) corresponding filter cake area；
S5, it is spatial point (t, r5, θ5) corresponding filter cake area；
riAnd θiWherein i=1,2,3,4,5, it is the radius and angle of corresponding two-dimensional surface polar coordinates point；
CM,i, it is spatial point (t, ri, θi) the corresponding miscellaneous concentration of metal ions of filter cake；
CM,P, it is the miscellaneous concentration of metal ions of filter cake overall average.
(6) case study on implementation of the miscellaneous concentration of metal ions of spatial point vs. of part detection is drawn in figure, further to dense
Du-when m- area data handled, can get corresponding miscellaneous tenor data, then by the data of a large amount of different mineral resources
It is integrated, large database concept can be established.
Standard Special sample taker in the step (2) are as follows: with the 316 stainless steel 25mm*2.5mm steel pipes of 40mm be sampling
Cylinder, external welding 200mm long 316 stainless steel solid rod Φ 6mm, a length of 20mm of weld seam.
The application of method described above in the white washing process characterization of titanium sulfate.
Beneficial effect
A kind of method for building up of the three-dimensional polar system of the titanium white washing Leaching Kinetics of characterization washing intensity, this method are established
Large database concept is washed, optimization titanium sulfate plain boiled water washes process conditions, reduces sulfuric acid titanium powder industry washing process water, reduces technique behaviour
Expenses and the human cost such as be used as power, and shortens metatitanic acid and washes the production cycle.
Detailed description of the invention
Fig. 1 is the two-dimentional polar coordinate system of simplified dimensionality reduction vacuum filtration blade.
Fig. 2 is the application specific standard sampler SXQY-5 that the present invention designs.
Fig. 3 is the case study on implementation figure of the miscellaneous concentration of metal ions of spatial point vs..
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
A kind of method for building up of the three-dimensional polar system of the titanium white washing Leaching Kinetics of characterization washing intensity, including following step
It is rapid:
(1) the two-dimentional polar coordinate system for simplifying the vacuum filtration blade of dimensionality reduction is constructed, each event is indicated with (t, r, θ), wherein t
The coordinate representation time；R coordinate representation is at a distance from pole；The angle of θ coordinate representation 0 ° of ray of coordinate distance counterclockwise；
See Fig. 1；
(2) it is sampled using the metatitanic acid filter cake that standard Special sample taker is formed for certain mineral resources, five different events (t,
ri, θi) wherein i=1,2,3,4,5,10g is sampled to washing metatitanic acid filter disc；
(3) it weighed, dried, 2h to above-mentioned sampling at a temperature of 120 DEG C；
(4) then using hydrochloric acid, sulfuric acid, nitric acid, perchloric acid, the one or more mixed acid of hydrobromic acid under the conditions of 200 DEG C of temperature
Resolution 1h is carried out to the sample dried in step (3), cooling, is settled to 1000ml；
(5) the miscellaneous concentration of metal ions that above-mentioned each constant volume solution is measured using flame atomic absorption spectrophotometer, calculates inclined titanium
Miscellaneous tenor in sour material；According to following formula to time point t1Corresponding heteroion concentration is calculated:
Wherein:
S1, it is spatial point (t, r1, θ1) corresponding filter cake area；
S2, it is spatial point (t, r2, θ2) corresponding filter cake area；
S3, it is spatial point (t, r3, θ3) corresponding filter cake area；
S4, it is spatial point (t, r4, θ4) corresponding filter cake area；
S5, it is spatial point (t, r5, θ5) corresponding filter cake area；
riAnd θiWherein i=1,2,3,4,5, it is the radius and angle of corresponding two-dimensional surface polar coordinates point；
CM,i, it is spatial point (t, ri, θi) the corresponding miscellaneous concentration of metal ions of filter cake；
CM,P, it is the miscellaneous concentration of metal ions of filter cake overall average.
Finally obtaining the miscellaneous concentration of metal ions data of the filter cake overall average is 47ppm.
(6) case study on implementation of the miscellaneous concentration of metal ions of spatial point vs. of part detection is drawn in figure, further to dense
Du-when m- area data handled, then the data of a large amount of different mineral resources are integrated, large database concept can be established.
Standard Special sample taker in the step (2) are as follows: with the 316 stainless steel 25mm*2.5mm steel pipes of 40mm be sampling
Cylinder, external welding 200mm long 316 stainless steel solid rod Φ 6mm, a length of 2mm of weld seam, as sampling handle.See Fig. 2.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (3)
1. a kind of method for building up of the three-dimensional polar system of the titanium white washing Leaching Kinetics of characterization washing intensity, feature exist
In, comprising the following steps:
(1) the two-dimentional polar coordinate system for simplifying the vacuum filtration blade of dimensionality reduction is constructed, each event is indicated with (t, r, θ), wherein t
The coordinate representation time；R coordinate representation is at a distance from pole；The angle of θ coordinate representation 0 ° of ray of coordinate distance counterclockwise；
(2) 0.1 is sampled to washing metatitanic acid filter disc for different events (t, r, θ) using standard Special sample taker ~
100g；
(3) it weighed, dried, 0.1 ~ 10h to above-mentioned sampling at a temperature of 0 ~ 120 DEG C；
(4) then using hydrochloric acid, sulfuric acid, nitric acid, perchloric acid, the one or more mixed acid of hydrobromic acid in 0 ~ 300 DEG C of temperature condition
Under 0.1 ~ 10h of resolution carried out to the sample dried in step (3), cooling, be settled to 10 ~ 1000ml；
(5) the miscellaneous concentration of metal ions that above-mentioned each constant volume solution is measured using flame atomic absorption spectrophotometer, calculates inclined titanium
Miscellaneous tenor in sour material；It is as follows to handle formula, certain time point t1Corresponding heteroion concentration calculation formula is as follows:
Wherein:
S1, it is spatial point (t, r1, θ1) corresponding filter cake area；
S2, it is spatial point (t, r2, θ2) corresponding filter cake area；
S3, it is spatial point (t, r3, θ3) corresponding filter cake area；
S4, it is spatial point (t, r4, θ4) corresponding filter cake area；
S5, it is spatial point (t, r5, θ5) corresponding filter cake area；
riAnd θiWherein i=1,2,3,4,5, it is the radius and angle of corresponding two-dimensional surface polar coordinates point；
CM,i, it is spatial point (t, ri, θi) the corresponding miscellaneous concentration of metal ions of filter cake；
CM,P, it is the miscellaneous concentration of metal ions of filter cake overall average；
(6) the miscellaneous concentration of metal ions of spatial point vs. by part detection is drawn in figure, further to Concentration-time-area number
According to being handled, it can get corresponding miscellaneous tenor data, then the data of a large amount of different mineral resources are integrated, can establish
Large database concept.
2. the method according to claim 1, wherein the standard Special sample taker in the step (2) are as follows: with
The 316 stainless steel 25mm*2.5mm steel pipes of 40mm are sampler barrel, outer ring corner of polishing, 316 stainless steel solid of external welding 200mm long
Rod Φ 6mm, a length of 20mm of weld seam.
3. application of the method described in a kind of one of claim 1-2 in the white washing process characterization of titanium sulfate.
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| CN201810753996.1A CN109085153B (en) | 2018-07-11 | 2018-07-11 | Method for establishing three-dimensional polar coordinate system of titanium dioxide washing leaching dynamics for representing washing strength |
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| CN201810753996.1A CN109085153B (en) | 2018-07-11 | 2018-07-11 | Method for establishing three-dimensional polar coordinate system of titanium dioxide washing leaching dynamics for representing washing strength |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101090983A (en) * | 2004-10-21 | 2007-12-19 | 安格洛操作有限公司 | Leaching process in the presence of hydrochloric acid for the recovery of a value metal from an ore |
| CN102564835A (en) * | 2012-01-09 | 2012-07-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Sample preparation method and detecting method for detecting impurities in titanyl sulfate solution |
| CN104925859A (en) * | 2014-03-21 | 2015-09-23 | 徐迪青 | Titanium dioxide production method |
| CN105754378A (en) * | 2016-03-23 | 2016-07-13 | 南召鑫泰钙业有限公司 | Calcium-based titanium dioxide and preparation process thereof |
| CN106892453A (en) * | 2017-03-30 | 2017-06-27 | 四川龙蟒钛业股份有限公司 | The method that washing filtrate is used for acidolysis leaching |
-
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- 2018-07-11 CN CN201810753996.1A patent/CN109085153B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101090983A (en) * | 2004-10-21 | 2007-12-19 | 安格洛操作有限公司 | Leaching process in the presence of hydrochloric acid for the recovery of a value metal from an ore |
| CN102564835A (en) * | 2012-01-09 | 2012-07-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Sample preparation method and detecting method for detecting impurities in titanyl sulfate solution |
| CN104925859A (en) * | 2014-03-21 | 2015-09-23 | 徐迪青 | Titanium dioxide production method |
| CN105754378A (en) * | 2016-03-23 | 2016-07-13 | 南召鑫泰钙业有限公司 | Calcium-based titanium dioxide and preparation process thereof |
| CN106892453A (en) * | 2017-03-30 | 2017-06-27 | 四川龙蟒钛业股份有限公司 | The method that washing filtrate is used for acidolysis leaching |
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