CN109085153B - Method for establishing three-dimensional polar coordinate system of titanium dioxide washing leaching dynamics for representing washing strength - Google Patents
Method for establishing three-dimensional polar coordinate system of titanium dioxide washing leaching dynamics for representing washing strength Download PDFInfo
- Publication number
- CN109085153B CN109085153B CN201810753996.1A CN201810753996A CN109085153B CN 109085153 B CN109085153 B CN 109085153B CN 201810753996 A CN201810753996 A CN 201810753996A CN 109085153 B CN109085153 B CN 109085153B
- Authority
- CN
- China
- Prior art keywords
- washing
- filter cake
- concentration
- titanium dioxide
- polar coordinate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/72—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flame burners
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
- G01N1/08—Devices for withdrawing samples in the solid state, e.g. by cutting involving an extracting tool, e.g. core bit
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
Abstract
The invention discloses a method for establishing a three-dimensional polar coordinate system of titanium dioxide washing leaching dynamics for representing washing strength. By the mode, the method makes up a blank point of the washing process for producing metatitanic acid from titanium white at present. The washing process conditions of the titanium sulfate white can be optimized, the washing process water in the titanium sulfate white industry is reduced, the cost such as process operation power and the like and the labor cost are reduced, and the washing production period of the metatitanic acid is shortened.
Description
Technical Field
The invention belongs to the technical field of titanium dioxide production by a sulfuric acid method, and particularly relates to a method for establishing a three-dimensional polar coordinate system of titanium dioxide washing leaching dynamics representing washing strength.
Background
Titanium dioxide (TiO) in the world at present2) The production process mainly comprises two processes of chlorination process titanium dioxide and sulfuric acid process titanium dioxide. The sulfuric acid method for producing titanium dioxide has already been in the history of 90 years, and has mature process route, low requirement on the strength of equipment and devices and low requirement on the grade of raw materials, and can produce titanium dioxide in two crystal forms of anatase and rutile at the same time, so far, the titanium dioxide sulfuric acid method still has strong activity and can be mutually supplemented with a chlorination method and coexist for a long time. The important raw material for producing titanium white by the sulfuric acid method is ilmenite (FeTiO)3) Typical content data based on X-ray fluorescence spectroscopy of domestic ilmenite are shown in Table 1 below.
TABLE 1 typical ilmenite X-ray fluorescence spectroscopy data (in oxides)
| Metallic element | TiO2 | Fe2O3 | Al2O3 | SiO2 | P2O5 | CaO | MgO | Cr2O3 |
| Mass fraction of% | 45.5 | 46.1 | 0.8 | 5.8 | 0.13 | 3.4 | 0.9 | 0.005 |
| Metallic element | MnO | V2O5 | ZrO2 | Nb2O5 | Na2O | ZnO | K2O | |
| Mass fraction of% | 1.2 | 0.04 | 0.049 | 0.02 | 0.109 | 0.012 | 0.09 |
The metatitanic acid (10H) is generated after the ilmenite is subjected to acidolysis, purification, concentration and hydrolysis2TiO3·SO3) A large amount of water-soluble metal hetero ions and sulfate radical and other anions are adsorbed, the existence of the hetero ions influences the calcining process and the quality of the final titanium dioxide, and therefore the hetero ions must be removed before the calcining process. At present, the titanium white industry adopts a washing impurity removal process, and the washing section consumes a large amount of process water, which is also an important reason that the titanium white sulfate industry is called as high water consumption industry. Most of manufacturers use a vacuum leaf filter as the water washing equipment in the working section, and the filter is composed of a plurality of groups of filter plates, so that the phenomenon of uneven washing of filter cakes is generally caused due to the inherent vacuum/suction filtration structure problem of the filter plates. The end point of the washing of the hydrolyzed material in different situations cannot be guided and dealt with by the ferrous iron content in the titration filtrate and the experience of first-line workers. Two problems tend to result: first, washingThe strength is insufficient, so that the impurity content is higher, and the final quality of the titanium dioxide is influenced. Secondly, the washing intensity is too big, leads to the water consumption to be more huge, simultaneously has the working costs and the human cost of vacuum pump.
At present, the solid-liquid extraction kinetics research of the metatitanic acid washing section in the titanium dioxide industry of the domestic sulfuric acid process aiming at the inherent structure of the filter plate of the leaf filter is obviously insufficient for different mineral powders and special accidental hydrolysis conditions, and the method is not only lack of theoretical support but also has no research means. The problem is related to the production cycle of the titanium white industry, the electric energy consumption of the washing section, the labor cost and especially the washing water consumption, which is a blank point of the metatitanic acid washing process of the titanium white enterprise at present.
Disclosure of Invention
The invention mainly solves the technical problem of providing the establishment method of the three-dimensional polar coordinate system of the titanium dioxide washing leaching dynamics for representing the washing strength, and makes up a blank point of the current titanium dioxide production metatitanic acid washing process.
The technical scheme adopted by the invention is as follows: aiming at the hydrolyzed materials of different ore species and operation conditions, a space-time point (t, r, theta) sample is semi-continuously collected by using a standard special sampler, the content of the impurity metal of the sample point (t, r, theta) at different time and space positions is measured by flame atomic absorption spectroscopy, a large database is constructed and analyzed, and a standardized water washing central control system is established.
A method for establishing a three-dimensional polar coordinate system of titanium dioxide washing leaching dynamics for representing washing strength comprises the following steps:
(1) constructing a two-dimensional polar coordinate system of the vacuum filtration blade with simplified dimension reduction, wherein each space-time point is represented by (t, r, theta), and the t coordinate represents time; the r coordinate represents the distance from the pole; the coordinate theta represents the angle of a ray from 0 degrees in a counterclockwise coordinate;
(2) sampling 0.1-100 g of the washing metatitanic acid filter cake by using a standard special sampler according to different time-space points (t, r, theta);
(3) weighing and drying the samples at the temperature of 0-120 ℃ for 0.1-10 hours;
(4) then, digesting the dried sample in the step (3) for 0.1-10 h by using one or more mixed acids of hydrochloric acid, sulfuric acid, nitric acid, perchloric acid and hydrobromic acid at the temperature of 0-300 ℃, cooling and fixing the volume to 10-1000 ml;
(5) measuring the concentration of the impurity metal ions of each constant volume solution by using a flame atomic absorption spectrophotometer, and calculating the content of the impurity metal in the metatitanic acid material; a typical processing equation is as follows, a certain point in time t1The corresponding calculation formula of the concentration of the hetero ions is as follows:
wherein:
S1is a spatial point (t, r)1，θ1) The corresponding filter cake area;
S2is a spatial point (t, r)2，θ2) The corresponding filter cake area;
S3is a spatial point (t, r)3，θ3) The corresponding filter cake area;
S4is a spatial point (t, r)4，θ4) The corresponding filter cake area;
S5is a spatial point (t, r)5，θ5) The corresponding filter cake area;
riand thetaiWherein i =1,2,3,4,5, which is the radius and angle of the polar coordinate point of the corresponding two-dimensional plane;
a hetero metal ion, a water-soluble metal hetero ion;
CM,iis a spatial point (t, r)i，θi) Corresponding filter cake heterometalion concentration, wherein i =1,2,3,4, 5;
CM,Pthe total average concentration of the impurity metal ions in the filter cake;
(6) And drawing the implementation case of the concentration of the partially detected space points vs. the concentration of the impurity metal ions in a graph, further processing the concentration-time-area data to obtain corresponding data of the content of the impurity metal, integrating a large amount of data of different mineral sources, and establishing a large database.
The standard special sampler in the step (2) is as follows: a40 mm 316 stainless steel 25mm 2.5mm steel pipe is used as a sampling cylinder, a 200mm long 316 stainless steel solid stick phi 6mm is welded outside, and the length of a welding line is 20 mm.
The method is applied to the characterization of the titanium sulfate white water washing process.
Advantageous effects
A method for establishing a three-dimensional polar coordinate system of titanium dioxide washing leaching dynamics for representing washing strength is characterized in that a washing large database is established, washing process conditions of titanium sulfate are optimized, washing process water in the titanium sulfate industry is reduced, cost such as process operation power and labor cost are reduced, and a metatitanic acid washing production period is shortened.
Drawings
FIG. 1 is a two-dimensional polar coordinate system of a simplified dimension-reducing vacuum filtration blade.
FIG. 2 is a special standard sampler SXQY-5, 1-sampling cylinder, 2-sampling handle.
Fig. 3 is a graph of an example of the concentration of the hetero-metal ions at a spatial point vs.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
A method for establishing a three-dimensional polar coordinate system of titanium dioxide washing leaching dynamics for representing washing strength comprises the following steps:
(1) constructing a two-dimensional polar coordinate system of the vacuum filtration blade with simplified dimension reduction, wherein each space-time point is represented by (t, r, theta), and the t coordinate represents time; the r coordinate represents the distance from the pole; the coordinate theta represents the angle of a ray from 0 degrees in a counterclockwise coordinate; see FIG. 1;
(2) using standard proprietary samplingThe device samples metatitanic acid filter cake formed by a certain mineral source, and five different time-space points (t, r)i，θi) Wherein i =1,2,3,4,5, 10g of the water-washed metatitanic acid cake was sampled;
(3) weighing the samples at 120 ℃, and drying for 2 hours;
(4) then, digesting the dried sample in the step (3) for 1h by using one or more mixed acids of hydrochloric acid, sulfuric acid, nitric acid, perchloric acid and hydrobromic acid at the temperature of 200 ℃, cooling and fixing the volume to 1000 ml;
(5) measuring the concentration of the impurity metal ions of each constant volume solution by using a flame atomic absorption spectrophotometer, and calculating the content of the impurity metal in the metatitanic acid material; for the time point t according to the following formula1The corresponding concentration of the hetero-ions was calculated:
wherein:
S1is a spatial point (t, r)1，θ1) The corresponding filter cake area;
S2is a spatial point (t, r)2，θ2) The corresponding filter cake area;
S3is a spatial point (t, r)3，θ3) The corresponding filter cake area;
S4is a spatial point (t, r)4，θ4) The corresponding filter cake area;
S5is a spatial point (t, r)5，θ5) The corresponding filter cake area;
riand thetaiWherein i =1,2,3,4,5, which is the radius and angle of the polar coordinate point of the corresponding two-dimensional plane;
a hetero metal ion, a water-soluble metal hetero ion;
CM,iis a spatial point (t, r)i，θi) Corresponding filter cake heterometalion concentration, wherein i =1,2,3,4, 5;
CM,Pthe total average concentration of the impurity metal ions in the filter cake;
The total average heterometal ion concentration data for this filter cake was finally obtained to be 47 ppm.
(6) And drawing the implementation case of the concentration of the impurity metal ions at the space points vs. the partial detection in a graph, further processing the concentration-time-area data, and integrating a large amount of data of different mineral sources to establish a large database.
The standard special sampler in the step (2) is as follows: a40 mm 316 stainless steel 25mm 2.5mm steel pipe is used as a 1-sampling cylinder, a 200mm long 316 stainless steel solid stick phi 6mm is welded outside, and a welding line is 2mm and used as a 2-sampling handle. See fig. 2.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (3)
1. A method for establishing a three-dimensional polar coordinate system of titanium dioxide washing leaching kinetics for representing washing strength is characterized by comprising the following steps:
(1) constructing a two-dimensional polar coordinate system of the vacuum filtration blade with simplified dimension reduction, wherein each space-time point is represented by (t, r, theta), and the t coordinate represents time; the r coordinate represents the distance from the pole; the coordinate theta represents the angle of a ray from 0 degrees in a counterclockwise coordinate;
(2) sampling 0.1-100 g of the washing metatitanic acid filter cake by using a standard special sampler according to different time-space points (t, r, theta);
(3) weighing and drying the samples at the temperature of 0-120 ℃ for 0.1-10 hours;
(4) then, digesting the dried sample in the step (3) for 0.1-10 h by using one or more mixed acids of hydrochloric acid, sulfuric acid, nitric acid, perchloric acid and hydrobromic acid at the temperature of 0-300 ℃, cooling and fixing the volume to 10-1000 ml;
(5) measuring the concentration of the impurity metal ions of each constant volume solution by using a flame atomic absorption spectrophotometer, and calculating the content of the impurity metal in the metatitanic acid material; the processing formula is as follows, a certain time point t1The corresponding calculation formula of the concentration of the hetero ions is as follows:
wherein:
S1is a spatial point (t, r)1，θ1) The corresponding filter cake area;
S2is a spatial point (t, r)2，θ2) The corresponding filter cake area;
S3is a spatial point (t, r)3，θ3) The corresponding filter cake area;
S4is a spatial point (t, r)4，θ4) The corresponding filter cake area;
S5is a spatial point (t, r)5，θ5) The corresponding filter cake area;
riand thetaiWherein i =1,2,3,4,5, which is the radius and angle of the polar coordinate point of the corresponding two-dimensional plane;
a hetero metal ion, a water-soluble metal hetero ion;
CM,iis a spatial point (t, r)i，θi) Corresponding filter cake heterometalion concentration, wherein i =1,2,3,4, 5;
CM,Pthe total average concentration of the impurity metal ions in the filter cake;
rL1/4 the length of the bottom edge of the filter plate;
(6) drawing the partially detected space points vs. the concentration of the impurity metal ions in a graph, further processing the concentration-time-area data to obtain corresponding impurity metal content data, integrating a large amount of data of different mineral sources, and establishing a large database.
2. The method of claim 1, wherein the standard dedicated sampler in step (2) is: a40 mm 316 stainless steel 25mm 2.5mm steel pipe is used as a sampling cylinder, the outer ring corner is polished, a 200mm long 316 stainless steel solid stick phi 6mm is welded outside, and the length of a welding line is 20 mm.
3. Use of the method according to any one of claims 1-2 for the characterization of a titanium dioxide sulfate water washing process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109085153A CN109085153A (en) | 2018-12-25 |
| CN109085153B true CN109085153B (en) | 2020-11-06 |
Family
ID=64837539
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810753996.1A Active 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 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109085153B (en) |
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 |
-
2018
- 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109085153A (en) | 2018-12-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104803415B (en) | A kind of method being prepared rutile by acid-dissolved titanium slag | |
| Li et al. | Solvent extraction of vanadium from a stone coal acidic leach solution using D2EHPA/TBP: Continuous testing | |
| CN104860347A (en) | Preparation method of artificial rutile | |
| Ye et al. | Recovery of vanadium from stone coal acid leaching solution by coprecipitation, alkaline roasting and water leaching | |
| CN105300975B (en) | The detection method of phosphorus content in a kind of vanadium slag | |
| CN108715938A (en) | A kind of technique improving the electric Zn system germanium rate of recovery | |
| CN109085153B (en) | Method for establishing three-dimensional polar coordinate system of titanium dioxide washing leaching dynamics for representing washing strength | |
| Shenxu et al. | Determination of vanadium valency in roasted stone coal by separate dissolve-potentiometric titration method | |
| CN105004711A (en) | Quantitative analysis method of impurities in beta-SiC | |
| CN105300974B (en) | The detection method of manganese content is aoxidized in a kind of vanadium slag | |
| CN107190155A (en) | Vanadium, the method for chromium are extracted in a kind of mixed liquor from containing vanadium and chromium | |
| CN1074542C (en) | Process for preparing solution for atomic absorption detecting total aluminium in iron and steel | |
| Yuan et al. | Source separation of V and Fe by two-stage selective leaching during V extraction from stone coal | |
| CN112694326A (en) | Zircon sand iron removal process | |
| CN102830154A (en) | Method for determining content of phosphor in ferrotungsten | |
| Mohammed et al. | Preparation of high-purity zirconia from Egyptian zircon: an anion-exchange purification process | |
| CN102636619A (en) | Method for measuring content of trace chloride ions in ferric oxide | |
| Liu et al. | The electrowinning of vanadium oxide from alkaline solution | |
| CN114751419A (en) | Process for preparing high-purity quartz sand by acid leaching purification | |
| CN111268730A (en) | Secondary recovery method of molybdenum in molybdate production process | |
| CN103962226B (en) | Calcining, alkali leaching, pickling and magnetic reconnection is utilized to close and select v-ti magnetite concentrate method again | |
| CN109085031B (en) | Method for determining Van der Waals adsorption organic matter of reduced iron powder in titanium white industry, and establishment and application of quality detection system thereof | |
| CN102168178A (en) | Method for extracting vanadium again from tailing after extracting vanadium from vanadium tailing of converter | |
| Wang et al. | Flotation behaviour and surface characteristic of anosovite in a sodium oleate solution | |
| CN116514132A (en) | Iron and titanium removing process for zircon sand |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |