CN113740479A - Method for qualitatively determining acidolysis rate degree of acid-ore mixture - Google Patents
Method for qualitatively determining acidolysis rate degree of acid-ore mixture Download PDFInfo
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- CN113740479A CN113740479A CN202110947569.9A CN202110947569A CN113740479A CN 113740479 A CN113740479 A CN 113740479A CN 202110947569 A CN202110947569 A CN 202110947569A CN 113740479 A CN113740479 A CN 113740479A
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- acidolysis
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- ore mixture
- acidolysis rate
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- 239000000203 mixture Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000002253 acid Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005903 acid hydrolysis reaction Methods 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000006228 supernatant Substances 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 238000009835 boiling Methods 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000001514 detection method Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 11
- 239000010936 titanium Substances 0.000 description 11
- 229910052719 titanium Inorganic materials 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 235000010215 titanium dioxide Nutrition 0.000 description 8
- 238000002386 leaching Methods 0.000 description 6
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 5
- 239000004408 titanium dioxide Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/02—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using precipitation
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for qualitatively determining the acidolysis rate degree of an acid-ore mixture, which comprises the following steps: (1) taking 20mL of the acid ore mixture after the acid hydrolysis is finished, and placing the mixture into a 500mL conical flask; (2) adding deionized water to 200mL, and boiling for 5 min; (3) adding water to 500mL, shaking up fully, standing for 2 min; (4) pouring 300mL of supernatant, adding water to 500mL, fully shaking, standing for 2min, pouring 300mL of supernatant, and repeating the steps for several times to obtain a to-be-detected substance; (5) and comparing the amount of the precipitate with the amount of the to-be-detected object by using the acid ore mixture with different acidolysis rates as a standard sample, so as to determine the acidolysis rate of the to-be-detected object. The invention has the beneficial effects of providing a simple, convenient, accurate and strong-timeliness acidolysis rate detection method, being capable of feeding back production in time to correspondingly adjust the acidolysis rate of the acid ore mixture, being strong-timeliness, being simple to operate and being short in operation time.
Description
Technical Field
The invention relates to the technical field of detection of acidolysis rate of ilmenite. In particular to a method for measuring the acidolysis rate of mixed titanium ore in the production process of titanium dioxide by a sulfuric acid method.
Background
In the prior art, most manufacturers in China adopt a sulfuric acid method to produce titanium dioxide, ilmenite is the most main raw material for producing titanium dioxide, and the utilization rate of the titanium dioxide resource by the production process can be directly mastered by the acidolysis rate of ilmenite in factories. Therefore, the acidolysis rate is an important index for controlling the production cost of the titanium white product, and the accuracy of the acidolysis rate plays an important guiding role in factory production and operation. In titanium white manufacturing enterprises, the method of measuring the acidolysis rate is generally to sample the leachate from the upper part of the acidolysis pot, filter and wash the leachate, and calculate the acidolysis rate by detecting the titanium content in the titanium solution and the residue, respectively.
Chinese patent publication No. CN102830200A discloses a method for detecting the acidolysis rate of a titanium-containing mineral, which comprises the following steps: analyzing chemical components of the titaniferous ore, and then determining the acid-ore ratio of acidolysis reaction; mixing a predetermined amount of titaniferous ore and concentrated sulfuric acid according to an acid-to-ore ratio to form a mixture; adding water into the mixture to dilute the concentrated sulfuric acid to 80-92% by mass; carrying out acidolysis reaction; after the acidolysis reaction is finished, curing to obtain a reaction product; leaching the reaction product under the condition of water bath; filtering, separating and leaching the obtained substance to obtain titanium liquid and residue, and calcining the residue; calculating the acidolysis rate according to formula 1, wherein formula 1 is: the acidolysis rate is mA/(mA + mB) × 100%.
For another example, chinese patent publication No. CN108414394A discloses a method for measuring the acidolysis rate of mixed titanium ore in the production process of titanium dioxide by a sulfuric acid process, comprising: detecting the grade of TiO2 of the ilmenite; adding concentrated sulfuric acid and ilmenite into an acidolysis pot, fully stirring, adding hydrolysis mother liquor, and diluting the concentrated sulfuric acid; after the acidolysis reaction is finished, obtaining a solid-phase substance, and after the solid-phase substance is cured, adding a leaching solution into an acidolysis pot to leach the acidolysis solid-phase substance; adding iron powder into an acidolysis pot for reduction reaction; sampling part of leaching solution in an acidolysis pot after reduction reaction is finished, carrying out suction filtration on the taken leaching solution to obtain titanium solution and residue, washing and drying the residue to constant weight, and detecting TiO in residue dry basis2Grade of (d); measuring the total volume of the leaching solution obtained in the acidolysis pot after the reduction reaction is finished; and (4) calculating the acidolysis rate.
The measurement of the mixed titanium ore acidolysis rate in the above patents is quantitative measurement, and the acidolysis rate needs to be calculated, and although the method is accurate, the method consumes a great amount of time and is inconvenient to operate.
Disclosure of Invention
The invention aims to solve the technical problems that the existing method for measuring the acidolysis rate of titanium ore needs to wait for a long time, has poor timeliness, and provides a method for qualitatively determining the acidolysis rate degree of an acid-ore mixture.
The technical scheme of the invention is as follows: a method for qualitatively determining the acidolysis rate degree of an acid ore mixture comprises the following steps: (1) taking 20mL of the acid ore mixture after the acid hydrolysis is finished, and placing the mixture into a 500mL conical flask; (2) adding deionized water to 200mL, and boiling for 5 min; (3) adding water to 500mL, shaking up fully, standing for 2 min; (4) pouring 300mL of supernatant, adding water to 500mL, fully shaking, standing for 2min, pouring 300mL of supernatant, and repeating the steps for several times to obtain a to-be-detected substance; (5) and comparing the amount of the precipitate with the amount of the to-be-detected object by using the acid ore mixture with different acidolysis rates as a standard sample, so as to determine the acidolysis rate of the to-be-detected object.
The acid mine mixtures with different acidolysis rates in the scheme comprise five acid mine mixtures with acidolysis rates of 90% -91%, 92% -93%, 94% -95%, 96% -97% and 98% -99%, and the acidolysis degrees of the five acid mine mixtures are defined as 2.5, 2.0, 1.5, 1.0 and 0.5.
The method has the advantages that the method is simple, convenient, accurate and strong in timeliness, calculation is not needed, the acidolysis rate of the acid ore mixture can be timely fed back to production to be correspondingly adjusted, timeliness is strong, operation is simple, and operation time is short.
Drawings
FIG. 1 is a photograph comparing an object to be examined with a standard sample having an acid-hydrolysis degree of 0.5 in the present invention;
FIG. 2 is a photograph comparing an object to be examined with a standard sample having an acid hydrolysis degree of qualitatively 1 according to the present invention;
FIG. 3 is a photograph comparing the specimen to be examined with a standard sample having an acid-hydrolysis degree of 1.5 in the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1: (1) taking 20mL of the acid ore mixture after the acid hydrolysis is finished, and placing the mixture into a 500mL conical flask; (2) adding deionized water to 200mL, and boiling for 5 min; (3) adding water to 500mL, shaking up fully, standing for 2 min; (4) pouring 300mL of supernatant, adding water to 500mL, fully shaking, standing for 2min, pouring 300mL of supernatant, and repeating for 4 times in sequence to obtain a to-be-detected substance; (5) the method comprises the steps of selecting five acid-ore mixtures with acidolysis rates of 90% -91%, 92% -93%, 94% -95%, 96% -97% and 98% -99% as standard samples, determining the acidolysis degrees of the five acid-ore mixtures to be 2.5, 2.0, 1.5, 1.0 and 0.5, comparing the amounts of black precipitates with an object to be detected, determining the range within which the acidolysis rate of the object to be detected falls, according to the requirement of target acidolysis rate, if the acidolysis rate of the object to be detected is lower than the target acidolysis rate, increasing the acidolysis rate of the acid-ore mixture where the object to be detected is located, and if the acidolysis rate of the object to be detected is higher than the target acidolysis rate, reducing the acidolysis rate of the acid-ore mixture where the object to be detected is located. As shown in FIG. 1, the test substance was found to be closest to the standard sample having an acid hydrolysis degree of 0.5 by comparison with five kinds of the standard samples, thereby determining the acid hydrolysis ratio of the test substance.
Example 2: the difference from example 1 is that the test substance was found to be closest to the standard sample of the acid hydrolysis degree 1 by comparing with five kinds of the standard samples as shown in FIG. 2, thereby determining the acid hydrolysis rate of the test substance.
Example 3: the difference from example 1 is that the acid hydrolysis rate of the specimen was determined by finding that it is closest to a standard sample having an acid hydrolysis degree of 1.5 by comparison with five standards as shown in FIG. 3.
The steps (1) to (4) of the invention are to add water or waste acid to extract the sampled ore pulp, remove the reacted titanium ore and finally precipitate the residual unreacted titanium slag, so that the result is closer to the actual value and the measurement is more accurate.
Claims (2)
1. A method for qualitatively determining the acidolysis rate degree of an acid ore mixture is characterized by comprising the following steps: the method comprises the following steps: (1) taking 20mL of the acid ore mixture after the acid hydrolysis is finished, and placing the mixture into a 500mL conical flask; (2) adding deionized water to 200mL, and boiling for 5 min; (3) adding water to 500mL, shaking up fully, standing for 2 min; (4) pouring 300mL of supernatant, adding water to 500mL, fully shaking, standing for 2min, pouring 300mL of supernatant, and repeating the steps for several times to obtain a to-be-detected substance; (5) and comparing the amount of the precipitate with the amount of the to-be-detected object by using the acid ore mixture with different acidolysis rates as a standard sample, so as to determine the acidolysis rate of the to-be-detected object.
2. The method for qualitatively determining the degree of acidolysis of an acid-ore mixture as claimed in claim 1, wherein: the acid ore mixture with different acidolysis rates comprises five acid ore mixtures with acidolysis rates of 90-91%, 92-93%, 94-95%, 96-97% and 98-99%, and the acidolysis degrees of the five acid ore mixtures are characterized as 2.5, 2.0, 1.5, 1.0 and 0.5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110947569.9A CN113740479A (en) | 2021-08-18 | 2021-08-18 | Method for qualitatively determining acidolysis rate degree of acid-ore mixture |
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| CN202110947569.9A CN113740479A (en) | 2021-08-18 | 2021-08-18 | Method for qualitatively determining acidolysis rate degree of acid-ore mixture |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636463A (en) * | 2012-04-24 | 2012-08-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Online detection device for titanyl sulfate hydrolysis and control equipment |
| CN102830200A (en) * | 2012-08-21 | 2012-12-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for detecting titanium-containing mineral acidolysis rate |
| CN106324184A (en) * | 2016-08-24 | 2017-01-11 | 云南冶金新立钛业有限公司 | Method for determining acidolysis rate of titanium slag |
| CN108414394A (en) * | 2018-06-13 | 2018-08-17 | 中国有色集团（广西）平桂飞碟股份有限公司 | The method that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate |
| CN110568123A (en) * | 2019-09-04 | 2019-12-13 | 广西蓝星大华化工有限责任公司 | Method for analyzing quality of titanium liquid after acidolysis leaching |
| CN111573719A (en) * | 2020-04-10 | 2020-08-25 | 安徽迪诺环保新材料科技有限公司 | Method for preparing high-surface-ratio and high-purity rutile type titanium dioxide by sulfuric acid process |
| CN113252418A (en) * | 2021-05-19 | 2021-08-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of sulfuric acid method titanium dioxide acidolysis solid-phase substance polished sample |
| CN113270150A (en) * | 2021-04-25 | 2021-08-17 | 安徽安纳达钛业股份有限公司 | Method for determining consistency of reaction acid concentration in titanium dioxide acidolysis |
-
2021
- 2021-08-18 CN CN202110947569.9A patent/CN113740479A/en active Pending
Patent Citations (9)
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| CN102636463A (en) * | 2012-04-24 | 2012-08-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Online detection device for titanyl sulfate hydrolysis and control equipment |
| EP2657688A1 (en) * | 2012-04-24 | 2013-10-30 | Pangang Group Panzhihua Iron & Steel Research Institute Co., Ltd. | Device for detecting hydrolysis of titanium oxysulfate in real-time and apparatus for controlling hydrolysis of titanium oxysulfate |
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| CN106324184A (en) * | 2016-08-24 | 2017-01-11 | 云南冶金新立钛业有限公司 | Method for determining acidolysis rate of titanium slag |
| CN108414394A (en) * | 2018-06-13 | 2018-08-17 | 中国有色集团（广西）平桂飞碟股份有限公司 | The method that sulfate process titanium dioxide production process measures mixing titanium ore acidolysis rate |
| CN110568123A (en) * | 2019-09-04 | 2019-12-13 | 广西蓝星大华化工有限责任公司 | Method for analyzing quality of titanium liquid after acidolysis leaching |
| CN111573719A (en) * | 2020-04-10 | 2020-08-25 | 安徽迪诺环保新材料科技有限公司 | Method for preparing high-surface-ratio and high-purity rutile type titanium dioxide by sulfuric acid process |
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