CN103540752B - One is scandium-enriched, titanium and vanadium and useless acid-treated method thereof from titanium dioxide waste acid by sulfuric acid process - Google Patents
One is scandium-enriched, titanium and vanadium and useless acid-treated method thereof from titanium dioxide waste acid by sulfuric acid process Download PDFInfo
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Abstract
A kind of from titanium dioxide waste acid by sulfuric acid process scandium-enriched, titanium and vanadium and useless acid-treated method thereof, comprise the steps: to carry out two sections of neutralizations with calcium carbonate to titanium white waste acid, obtain white gypsum and be enriched scandium, in two sections of vanadium titanium and slag; Carry out stripping with slag titanium white waste acid in two sections, dissolution fluid is carried out to the extraction and back-extraction of scandium, obtain thick scandium slag; More than extraction scandium, liquid carries out the hydrolysis of titanium, obtains titanium slag; During hydrolysis filtrate is carried out with sodium carbonate and precipitation, obtain vanadium slag, after precipitation liquid and two sections of neutralization filtrates in the lump through aeration and further neutralize after qualified discharge.The present invention can scandium-enriched, titanium and vanadium from titanium white waste acid effectively, spent acid tail washings qualified discharge after treatment.
Description
Technical field
The present invention relates to one scandium-enriched, titanium and vanadium and useless acid-treated method thereof from titanium dioxide waste acid by sulfuric acid process.
Background technology
At present, the administering method of titanium dioxide waste acid by sulfuric acid process mainly contains rhombspar up-flow expansion neutralisation, limestone vegetation method, and worldwide sulfuric acid method titanium pigment factory owner will adopt the method for similar limestone vegetation.In addition, domestic and international many manufacturers and scientific research personnel once proposed products such as spent acid and ore effect Sulphuric acid manganese, Tai-Ace S 150, zinc sulfate, but these process means all exist that ore effective constituent leaching yield is low, solid-liquid separation is more difficult, poor product quality, cause secondary pollution problems.
Except containing except a large amount of sulfuric acid and iron in titanium dioxide waste acid by sulfuric acid process, still there are the valuable metals such as scandium, vanadium and titanium, while environment protection treating is carried out to spent acid, carry out the synthetical recovery of scandium, vanadium and titanium, meet the principle of industrial effluent improvement and recycling.In order to extract the Scium trioxide in spent acid, forefathers have done a lot of work, but its technique is direct organic extraction, but overall extraction cost is higher.Extract in titanium white waste acid in vanadium, what Ishihara Sangyo Kaisha, Ltd. of Japan utilized is in ammonia and sintering leaching technology prepares ammonium meta-vanadate, this cover waste acid treatment technique it is reported and realizes industrialization, but due to its technological process too complex, the middle-size and small-size titanium powder plant of China is difficult to imitate.And directly from titanium white waste acid, extract the research of titanium at present there are no relevant report.
Summary of the invention
For the problems referred to above, the object of this invention is to provide one scandium-enriched, titanium and vanadium and useless acid-treated method thereof from titanium dioxide waste acid by sulfuric acid process, the method can carry out environment protection treating to titanium white waste acid effectively, tail washings qualified discharge, the Sync enrichment wherein valuable metal such as scandium, vanadium and titanium, both the requirement having met environmental protection also achieves the recycling of titanium white waste acid, particularly improves the extraction process of scandium, reduces the extraction cost of scandium.
The present invention realizes above-mentioned purpose by following technical solution: one is scandium-enriched, titanium and vanadium and useless acid-treated method thereof from titanium dioxide waste acid by sulfuric acid process, comprises the following steps:
1, carry out one section of neutralization with calcium carbonate to titanium white waste acid, reaction end pH value controls 1.0 ~ 2.0, obtains one section of neutralization filtrate and white gypsum after filtration.
2, with calcium carbonate, two sections of neutralizations are carried out to one section and filtrate again, reaction end pH value controls 4.0 ~ 5.0, must be enriched in scandium, vanadium and titanium two sections after filtration and slag, the dilute acid pretreatment system that two sections of neutralization filtrates deliver to titanium powder plant carries out aeration and further neutralizing treatment, and tail washings reaches GB8978-1996 discharge.
3, by two sections and slag H
+concentration is that the titanium white waste acid of 4.0 ~ 6.0g/L carries out stripping, and liquid-solid volume and weight ratio are 1.0 ~ 3.0, obtain dissolution fluid and GYPSUM RUBRUM after filtration.
4, dissolution fluid is carried out to the extracting operation of scandium, extraction agent composition is P204+TBP+ sulfonated kerosene, O/A=1:5 ~ 1:10, extraction time 5 ~ 10min, counter-current extraction, and extraction progression is 2 grades.Scandium percentage extraction is 95% ~ 99%.
5, carry out back extraction operation to negative scandium organic phase, reverse-extraction agent concentration is the NaOH of 1.5 ~ 2.5mol/L, and Stripping times is 20 ~ 30min, and back extraction progression is 1 grade, and the back extraction ratio of scandium is 98% ~ 100%.After back extraction gained thick scandium slag in Sc
2o
3content is 1 ~ 5%.
6, heating hydrolysis titanium is carried out to liquid more than extraction scandium, in whipping process, add crystal seed, keep solution boiling state 2.0 ~ 3.0h, after filtration, obtain titanium slag and hydrolysis filtrate.TiO in titanium slag
2content is 80% ~ 90%.
7, in carrying out with sodium carbonate hydrolysis filtrate and precipitation, reaction end pH value is 4.0 ~ 5.0, after filtration the solution after vanadium slag and precipitation, the solution after precipitation converges to two sections of neutralization filtrates handles together.V in vanadium slag
2o
5content be 1 ~ 3%.
The present invention compared with prior art has following beneficial effect:
1, the titanium dioxide waste acid by sulfuric acid process pH value after process of the present invention, close to neutral, get final product qualified discharge after the dilute acid pretreatment system recycling each titanium powder plant carries out simple aeration and further neutralizing treatment, achieves the thorough environment protection treating to titanium dioxide waste acid by sulfuric acid process.
2, the scandium in titanium white waste acid, vanadium and titanium are enriched 4 ~ 6 times, in titanium dioxide waste acid by sulfuric acid process, the low cost synthetical recovery of scandium, vanadium and titanium creates condition.
3, scandium owing to extracting in raw aqueous acid after enrichment again, compared with traditional direx process, reduces extraction cost.
4, the by product produced is white gypsum and a small amount of GYPSUM RUBRUM, and white gypsum is by being widely used as gypsum raw material or the building materials raw material of Cement industry use after dehydration and modification, a small amount of GYPSUM RUBRUM can be used as building materials raw material.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of scandium-enriched, titanium and vanadium and useless acid-treated method thereof from titanium dioxide waste acid by sulfuric acid process of the present invention.
Fig. 2 be of the present invention from titanium dioxide waste acid by sulfuric acid process in scandium-enriched, titanium and vanadium and useless acid-treated method thereof two sections and slag extract the process flow sheet of scandium, vanadium and titanium.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described.
Embodiment 1
As shown in Figure 1 and Figure 2, of the present invention from titanium dioxide waste acid by sulfuric acid process scandium-enriched, titanium and vanadium and useless acid-treated method thereof, comprise the following steps:
H is added in the retort of 200L
+concentration is the titanium white waste acid 100L of 5.92mol/L, wherein Sc
2o
3content is 32.8mg/L, V
2o
5content is 1.00g/L, TiO
2content is 7.00g/L, and add 30kg calcium carbonate and carry out one section of neutralization, reaction end pH value is 1.0 ~ 2.0, obtains one section of neutralization filtrate and white gypsum after press filtration and twice washing, Sc in one section of neutralization filtrate
2o
3content is 16.74mg/L, V
2o
5content is 0.52g/L, TiO
2content is 3.7g/L.This step Sc
2o
3, V
2o
5and TiO
2the rate of recovery be respectively 86.76%, 88.4% and 89.86%.
Add in one section of neutralization filtrate 3kg calcium carbonate to carry out in two sections and, reaction end pH value is 4.0 ~ 5.0, after press filtration in two sections and slag and two sections of neutralization filtrates, Sc in two sections and in slag
2o
3content is 0.04%, V
2o
5content is 1.24%, TiO
2content is 8.7%.Two sections of neutralization filtrates reach GB8978-1996 discharge after aeration and further neutralizing treatment.This step Sc
2o
3, V
2o
5and TiO
2the rate of recovery be respectively 97.93%, 97.73% and 96.36%.
By in two sections and slag H
+concentration is that the titanium white waste acid of 5.92mol/L dissolves, after press filtration and twice pickling, obtain dissolution fluid and GYPSUM RUBRUM.Sc in dissolution fluid
2o
3content is 156mg/L, V
2o
5content is 4.78g/L, TiO
2content is 34.12g/L.This step Sc
2o
3, V
2o
5and TiO
2the rate of recovery be respectively 97.26%, 96.26% and 98.44%.
By the organic phase of P204+TBP+ sulfonated kerosene and dissolution fluid to be in a ratio of O/A=1:5 ~ 1:10 to carry out scandium 2 stage countercurrent extracting operations by extraction tank, after phase-splitting, obtain liquid more than the organic phase of load scandium and extraction scandium.The organic phase concentration of load scandium is that the NaOH of 2.0mol/L carries out 1 grade of back extraction operation, obtains Sc
2o
3content is the thick scandium slag of 2.02%.The percentage extraction of this step scandium is 98.86%, and back extraction ratio is 98.5%.
Liquid more than extraction scandium is heated to seethe with excitement and is incubated 2 ~ 3h, after filtration, obtains hydrolysis filtrate and titanium slag.TiO in titanium slag
2content is 85%, V in hydrolysis filtrate
2o
5content is 4.55g/L, TiO
2content is 1.22g/L.The percent hydrolysis of this step titanium is 96.19%.
Add sodium carbonate and pH4.0 ~ 5.0 are neutralized to hydrolysis filtrate, obtain liquid after vanadium slag and precipitation after filtration, V in vanadium slag
2o
5content is 2.26%, and after precipitation, liquid converges and reach effluent standard after two sections of neutralization filtrates are handled together.The rate of recovery of this step vanadium is 98.68%.
The method process titanium white waste acid is thick scandium slag, vanadium slag and titanium slag extremely, Sc
2o
3, V
2o
5and TiO
2direct yield be respectively 80.9%, 76.78% and 74.74%.
Embodiment 2
The titanium white waste acid 100L that H+ concentration is 5.51mol/L is added, wherein Sc in the retort of 200L
2o
3content is 24.5mg/L, V
2o
5content is 0.87g/L, TiO
2content is 6.76g/L, and add 27kg calcium carbonate and carry out one section of neutralization, reaction end pH value is 1.0 ~ 2.0, obtains one section of neutralization filtrate and white gypsum after press filtration and twice washing, Sc in one section of neutralization filtrate
2o
3content is 12.52mg/L, V
2o
5content is 0.46g/L, TiO
2content is 3.52g/L.This step Sc
2o
3, V
2o
5and TiO
2the rate of recovery be respectively 88.67%, 89.89% and 88.52%.
Add in one section of neutralization filtrate 2.7kg calcium carbonate to carry out in two sections and, reaction end pH value is 4.0 ~ 5.0, after press filtration in two sections and slag and two sections of neutralization filtrates, Sc in two sections and in slag
2o
3content is 0.032%, V
2o
5content is 1.17%, TiO
2content is 8.9%.Two sections of neutralization filtrates reach GB8978-1996 discharge after aeration and further neutralizing treatment.This step Sc
2o
3, V
2o
5and TiO
2the rate of recovery be respectively 97.52%, 97.05% and 96.47%.
The titanium white waste acid in two sections with slag H+ concentration being 5.51mol/L is dissolved, after press filtration and twice pickling, obtains dissolution fluid and GYPSUM RUBRUM.Sc in dissolution fluid
2o
3content is 132mg/L, V
2o
5content is 4.72g/L, TiO
2content is 36.8g/L.This step Sc
2o
3, V
2o
5and TiO
2the rate of recovery be respectively 98.4%, 96.39% and 98.87%.
By the organic phase of P204+TBP+ sulfonated kerosene and dissolution fluid to be in a ratio of O/A=1:5 ~ 1:10 to carry out scandium 2 stage countercurrent extracting operations by extraction tank, after phase-splitting, obtain liquid more than the organic phase of load scandium and extraction scandium.The organic phase concentration of load scandium is that the NaOH of 2.0mol/L carries out 1 grade of back extraction operation, obtains Sc
2o
3content is the thick scandium slag of 1.75%.The percentage extraction of this step scandium is 98.8%, and back extraction ratio is 97.9%.
Liquid more than extraction scandium is heated to seethe with excitement and is incubated 2 ~ 3h, after filtration, obtains hydrolysis filtrate and titanium slag.TiO in titanium slag
2content is 86%, V in hydrolysis filtrate
2o
5content is 4.43g/L, TiO
2content is 1.1g/L.The percent hydrolysis of this step titanium is 96.81%.
Add sodium carbonate and pH4.0 ~ 5.0 are neutralized to hydrolysis filtrate, obtain liquid after vanadium slag and precipitation after filtration, V in vanadium slag
2o
5content is 2.16%, and after precipitation, liquid converges and reach effluent standard after two sections of neutralization filtrates are handled together.The rate of recovery of this step vanadium is 98.87%.
The method process titanium white waste acid is thick scandium slag, vanadium slag and titanium slag extremely, Sc
2o
3, V
2o
5and TiO
2direct yield be respectively 80.01%, 76.66% and 74.87%.
Embodiment 3
H is added in the retort of 200L
+concentration is the titanium white waste acid 100L of 4.49mol/L, wherein Sc
2o
3content is 13.5mg/L, V
2o
5content is 0.6g/L, TiO
2content is 3.9g/L, and add 22kg calcium carbonate and carry out one section of neutralization, reaction end pH value is 1.0 ~ 2.0, obtains one section of neutralization filtrate and white gypsum after press filtration and twice washing, Sc in one section of neutralization filtrate
2o
3content is 6.95mg/L, V
2o
5content is 0.31g/L, TiO
2content is 2.0g/L.This step Sc
2o
3, V
2o
5and TiO
2the rate of recovery be respectively 87.52%, 87.83% and 87.18%.
Add in one section of neutralization filtrate 2.2kg calcium carbonate to carry out in two sections and, reaction end pH value is 4.0 ~ 5.0, after press filtration in two sections and slag and two sections of neutralization filtrates, Sc in two sections and in slag
2o
3content is 0.0219%, V
2o
5content is 0.98%, TiO
2content is 6.3%.Two sections of neutralization filtrates reach GB8978-1996 discharge after aeration and further neutralizing treatment.This step Sc
2o
3, V
2o
5and TiO
2the rate of recovery be respectively 97.97%, 98.28% and 97.93%.
By in two sections and slag H
+concentration is that the titanium white waste acid of 4.49mol/L dissolves, after press filtration and twice pickling, obtain dissolution fluid and GYPSUM RUBRUM.Sc in dissolution fluid
2o
3content is 79.2mg/L, V
2o
5content is 3.55g/L, TiO
2content is 23.4g/L.This step Sc
2o
3, V
2o
5and TiO
2the rate of recovery be respectively 96.49%, 96.82% and 99.56%.
By the organic phase of P204+TBP+ sulfonated kerosene and dissolution fluid to be in a ratio of O/A=1:5 ~ 1:10 to carry out scandium 2 stage countercurrent extracting operations by extraction tank, after phase-splitting, obtain liquid more than the organic phase of load scandium and extraction scandium.The organic phase concentration of load scandium is that the NaOH of 2.0mol/L carries out 1 grade of back extraction operation, obtains Sc
2o
3content is the thick scandium slag of 1.67%.The percentage extraction of this step scandium is 98.26%, and back extraction ratio is 98.4%.
Liquid more than extraction scandium is heated to seethe with excitement and is incubated 2 ~ 3h, after filtration, obtains hydrolysis filtrate and titanium slag.TiO in titanium slag
2content is 84.3%, V in hydrolysis filtrate
2o
5content is 3.35g/L, TiO
2content is 0.95g/L.The percent hydrolysis of this step titanium is 95.68%.
Add sodium carbonate and pH4.0 ~ 5.0 are neutralized to hydrolysis filtrate, obtain liquid after vanadium slag and precipitation after filtration, V in vanadium slag
2o
5content is 1.58%, and after precipitation, liquid converges and reach effluent standard after two sections of neutralization filtrates are handled together.The rate of recovery of this step vanadium is 99.1%.
The method process titanium white waste acid is thick scandium slag, vanadium slag and titanium slag extremely, Sc
2o
3, V
2o
5and TiO
2direct yield be respectively 80.9%, 77.07% and 74.76%.
Claims (1)
1. a scandium-enriched from titanium dioxide waste acid by sulfuric acid process, titanium and vanadium and useless acid-treated method thereof, comprise, with calcium carbonate, one section of neutralization is carried out to titanium white waste acid, reaction end pH value controls 1.0 ~ 2.0, obtain one section of neutralization filtrate and white gypsum after filtration and with calcium carbonate, two sections of neutralizations carried out to one section of neutralization filtrate, reaction end pH value controls 4.0 ~ 5.0, obtain being enriched in scandium, vanadium and titanium two sections after filtration and slag and two sections of neutralization filtrate steps, it is characterized in that, also comprise the following steps:
(1) the dilute acid pretreatment system two sections of neutralization filtrates being delivered to titanium powder plant carries out aeration and further neutralizing treatment, tail washings GB8978-1996 discharge up to standard;
(2) by two sections and slag H
+concentration is that the titanium white waste acid of 4.0 ~ 6.0g/L carries out stripping, and liquid-solid volume and weight ratio are 1.0 ~ 3.0, obtain dissolution fluid and GYPSUM RUBRUM after filtration;
(3) carry out extracting scandium to dissolution fluid, extraction agent is P204+TBP+ sulfonated kerosene, is in a ratio of O/A=1:5 ~ 1:10, extraction time 5 ~ 10min, counter-current extraction, and extraction progression is 2 grades;
(4) carry out back extraction to the organic phase of load scandium, reverse-extraction agent concentration is the NaOH of 1.5 ~ 2.5mol/L, and Stripping times is 20 ~ 30min, and back extraction progression is 1 grade;
(5) heating hydrolysis titanium is carried out to liquid more than extraction scandium, in whipping process, add crystal seed, keep solution boiling state 2.0 ~ 3.0h, after filtration, obtain titanium slag and hydrolysis filtrate;
(6) in carrying out with sodium carbonate hydrolysis filtrate and precipitation, reaction end pH value is 4.0 ~ 5.0, after filtration the solution after vanadium slag and precipitation, the solution after precipitation and two sections of neutralization filtrates are handled together.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023274838A1 (en) * | 2021-06-30 | 2023-01-05 | G S A (Environmental) Limited | PROCESS FOR THE RECOVERY OF RARE EARTH METALS FROM WASTE RESIDUES FROM TiO2 PRODUCTION |
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