CN103553123B - The bleaching method of metatitanic acid in a kind of Titanium White Production By Sulfuric Acid Process - Google Patents
The bleaching method of metatitanic acid in a kind of Titanium White Production By Sulfuric Acid Process Download PDFInfo
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- CN103553123B CN103553123B CN201310491257.7A CN201310491257A CN103553123B CN 103553123 B CN103553123 B CN 103553123B CN 201310491257 A CN201310491257 A CN 201310491257A CN 103553123 B CN103553123 B CN 103553123B
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- metatitanic acid
- sulfuric acid
- titanium white
- acid
- metatitanic
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Abstract
The present invention relates to the production field of titanium dioxide, particularly relate to the bleaching method of metatitanic acid in a kind of Titanium White Production By Sulfuric Acid Process, comprising: step one, will containing Fe
3+impurity add in reactor through washing qualified metatitanic acid, add water after stirring, then add industrial sulphuric acid; Step 2, EDTA-2Na is added in the metatitanic acid slurry of step one, keep temperature in reactor between 40 ~ 45 DEG C; Step 3, the metatitanic acid slurry cooling that step 2 is obtained, vacuum filtration, washing.The invention provides a kind of technique simple, be easy to realize, the bleaching method of metatitanic acid in sulfuric acid dosage is few, service temperature is low, bleaching time is short, noresidue pollution, bleaching effect are good Titanium White Production By Sulfuric Acid Process.
Description
Technical field
The present invention relates to the production field of titanium dioxide, particularly relate to the bleaching method of metatitanic acid in a kind of Titanium White Production By Sulfuric Acid Process.
Background technology
In current Titanium White Production By Sulfuric Acid Process, the bleaching method of metatitanic acid mainly contains zinc powder bleaching, aluminium powder bleaching, titanous bleaching, electric bleaching and in metatitanic acid slurry, first adds ionogenic surfactant, then adds metal-powder and do the method that reductive agent carries out bleaching.Industrial normal employing aluminium powder bleaching and titanous bleach this two kinds of methods.Wherein the bleaching of titanous is relatively good, and reason is compared with trivalent titanium solution bleaching is bleached with zinc powder or aluminium powder, the advantage such as have that sulfuric acid dosage is few, reductive agent consumption is few, service temperature is low, bleaching time is short, noresidue pollution, bleaching effect are good.But the preparation of trivalent titanium solution needs increase equipment and increases preparation workload, and preparation process is complicated, and during preparation, energy consumption is high, and acid consumption is large, and cost is high, and operating process is with danger simultaneously.
In industrial production the bleaching of metatitanic acid generally experience acid-soluble → reduction → washing three processes, wherein " reduction " play conclusive effect, make Fe by adding zinc powder, aluminium powder or titanous liquid
3+be reduced into Fe
2+, the present invention utilizes EDTA-2Na and Fe
3+the feature of easy complexing, adopts complexing bleaching to substitute reduction process, the ferric ion in solution and EDTA-2Na is reacted and generates high iron complex soluble in water, then through washing, remove high iron complex, thus reach the object of bleaching.
Summary of the invention
For above-mentioned technical problem, the present invention has designed and developed the bleaching method of metatitanic acid in a kind of Titanium White Production By Sulfuric Acid Process, object be to provide a kind of technique simple, be easy to realize, the bleaching method of metatitanic acid in sulfuric acid dosage is few, service temperature is low, bleaching time is short, noresidue pollution, bleaching effect are good Titanium White Production By Sulfuric Acid Process.
Technical scheme provided by the invention is:
A bleaching method for metatitanic acid in Titanium White Production By Sulfuric Acid Process, comprises the following steps:
Step one, will containing Fe
3+impurity add in reactor through washing qualified metatitanic acid, add water after stirring, then add industrial sulphuric acid;
Step 2, EDTA-2Na is added in the metatitanic acid slurry of step one, keep temperature in reactor between 40 ~ 45 DEG C;
Step 3, the metatitanic acid slurry cooling that step 2 is obtained, vacuum filtration, washing.
Preferably, in described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, in described step 2, by EDTA-2Na:Fe
3+add in the metatitanic acid slurry of step one with mol ratio 2 ~ 4:1 gradation under whipped state.
Preferably, in described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, in described step 2, continue heating makes the temperature in reactor be incubated 1 ~ 1.5h at 40 ~ 45 DEG C.
Preferably, in described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, add industrial sulphuric acid in described step one and make the sulfuric acid concentration of metatitanic acid slurry between 35 ~ 45g/L.
Preferably, in described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, in described step one in metatitanic acid slurry containing TiO
2between 235 ~ 245g/L.
Preferably, in described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, in described step one, pass in reactor and be steam heated to 40 ~ 45 DEG C.
Preferably, in described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, in described step 3 with water coolant by metatitanic acid slurry cool to room temperature.
Preferably, in described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, filter metatitanic acid slurry by the leaf filter midge with negative pressure of vacuum in described step 3.
Preferably, in described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, wash metatitanic acid with sand filter water in described step 3.
In Titanium White Production By Sulfuric Acid Process of the present invention, the beneficial effect of the bleaching method of metatitanic acid is: adopt the Fe in EDTA-2Na complexing bleaching metatitanic acid
3+, technique is simple, be easy to realize, sulfuric acid dosage is few, service temperature is low, bleaching time is short, noresidue pollution, bleaching effect are good, obtains TiO through washing, Ficus caricaL, calcining with after beating powder
2product whiteness is good, tinting strength is high, good dispersity, strong covering power.
Accompanying drawing explanation
Fig. 1 is the bleaching method schema of metatitanic acid in Titanium White Production By Sulfuric Acid Process of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail, can implement according to this with reference to specification sheets word to make those skilled in the art.
As shown in Figure 1, the invention provides the bleaching method of metatitanic acid in a kind of Titanium White Production By Sulfuric Acid Process, comprise the following steps:
Step one, will containing Fe
3+impurity add in reactor through washing qualified metatitanic acid, add water after stirring, then add industrial sulphuric acid, make hydroxide high ferro be dissolved as ferric sulphate solution, its reaction formula is as follows:
2Fe(OH)
3+3H
2SO
4=Fe
2(SO
4)
3+6H
2O；
Step 2, added by EDTA-2Na in the metatitanic acid slurry of step one, keep temperature in reactor between 40 ~ 45 DEG C, ferric sulphate and complex compound EDTA-2Na are reacted completely, generates corresponding high iron complex, the reaction formula that complexing is bleached is as follows:
Fe
3++HY
3-→FeY
-+H
+
Fe
3++H
2Y
2-→FeY
-+2H
+
Fe
3++H
3Y
-→FeY
-+3H
+
Complex reaction is successive processes, and HY
3-, H
2y
2-and H
3y
-exist in an acidic solution, they and Fe simultaneously
3+continuous complexing, generates H
+, cause Fe
3+solubility rate accelerate, and hydroxide high ferro and industrial sulphuric acid react in H
+rate of consumption is greater than H in complex reaction
+production rate, therefore H
+concentration reduces, Ti
4+solubility rate decline;
Step 3, metatitanic acid slurry cooling step 2 obtained, vacuum filtration, washing, washes away high iron complex, further to reduce the content of iron.
In described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, in described step 2, by EDTA-2Na:Fe
3+add in the metatitanic acid slurry of step one with mol ratio 2 ~ 4:1 gradation under whipped state.
In described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, in described step 2, continue heating makes the temperature in reactor be incubated 1 ~ 1.5h at 40 ~ 45 DEG C.
In described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, add industrial sulphuric acid in described step one and make the sulfuric acid concentration of metatitanic acid slurry between 35 ~ 45g/L.
In described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, in described step one in metatitanic acid slurry containing TiO
2between 235 ~ 245g/L.
In described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, in described step one, pass in reactor and be steam heated to 40 ~ 45 DEG C.
In described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, in described step 3 with water coolant by metatitanic acid slurry cool to room temperature.
In described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, filter metatitanic acid slurry by the leaf filter midge with negative pressure of vacuum in described step 3.
In described Titanium White Production By Sulfuric Acid Process metatitanic acid bleaching method in, wash metatitanic acid with sand filter water in described step 3.
Embodiment 1
Step one, in the enamel reactor with the chuck heating of stirring, add washing qualified metatitanic acid and water, the Trace Iron impurity of metatitanic acid is with Fe
2o
3meter content is 0.010%, stirs and adjusts in metatitanic acid slurry containing TiO
2for 235g/L, then add a certain amount of industrial sulphuric acid, make the sulfuric acid concentration of metatitanic acid slurry be 35g/L, lead to and be steam heated to 40 DEG C, make hydroxide high ferro be dissolved as ferric sulphate solution;
Step 2, by EDTA-2Na/Fe
3+mol ratio is 4:1 meter, and take complexing agent EDTA-2Na and the furnishing solution that adds water, under whipped state, gradation adds in metatitanic acid slurry, continue heating, make temperature be incubated 1.5h at 40 DEG C, ferric sulphate and complex compound EDTA-2Na are reacted completely, generates corresponding high iron complex;
Step 3, by complexing bleach after metatitanic acid slurry lead to water quench to room temperature, filter by the leaf filter midge with negative pressure of vacuum, then with sand filter water washing metatitanic acid slurry, wash away high iron complex further, to reduce the content of iron, until Fe in metatitanic acid slurry
2o
3content be qualified lower than 0.003%, the metatitanic acid slurry after washing is through Ficus caricaL, calcining and the PGA100 type titanium dioxide product made after beating powder, and the performance index of this product are as shown in table 1.
Table 1 embodiment 1 product performance index
Embodiment 2
Step one, in the enamel reactor with the chuck heating of stirring, add washing qualified metatitanic acid and water, the Trace Iron impurity of metatitanic acid is with Fe
2o
3meter content is 0.008%, stirs and adjusts in metatitanic acid slurry containing TiO
2for 245g/L, then add a certain amount of industrial sulphuric acid, make the sulfuric acid concentration of metatitanic acid slurry be 45g/L, lead to and be steam heated to 45 DEG C, make hydroxide high ferro be dissolved as ferric sulphate solution;
Step 2, by EDTA-2Na/Fe
3+mol ratio is 3:1 meter, and take complexing agent EDTA-2Na and the furnishing solution that adds water, under whipped state, gradation adds in metatitanic acid slurry, continue heating, make temperature be incubated 1h at 45 DEG C, ferric sulphate and complex compound EDTA-2Na are reacted completely, generates corresponding high iron complex;
Step 3, by complexing bleach after metatitanic acid slurry lead to water quench to room temperature, filter by the leaf filter midge with negative pressure of vacuum, then with sand filter water washing metatitanic acid slurry, wash away high iron complex further, to reduce the content of iron, until Fe in metatitanic acid slurry
2o
3content be qualified lower than 0.003%, the metatitanic acid slurry after washing is through Ficus caricaL, calcining and the PGA100 type titanium dioxide product made after beating powder, and the performance index of this product are as shown in table 2.
Table 2 embodiment 2 product performance index
Table 3 is the comparing result of PGA100 type titanium dioxide and the GB/T1706-2006 product performance index adopting method of the present invention to obtain.Can find out, the PGA100 type titanium dioxide obtained by method of the present invention, product performance are equivalent to the high-grade titanium dioxide of Japanese A100, Korea S K100 series, performance index are better than GB/T1706-2006, this produce market selling price compared with A1 type product, increase per ton 500 yuan of sales revenue.
Table 3 product performance index comparing result
| Name index claims | GB/T1706-2006A1 type | PGA100 |
| TiO 2Content % | ≥98.0 | ≥98.3 |
| Color (with standard ratio) | Approximate | |
| Reducing power % | ≥103 | |
| Water solubles % | ≤0.6 | ≤0.5 |
| PH value | 6.5-8.0 | |
| Oil number g/100g sample | ≤24 | |
| 45 μm of screenings % | ≤0.1 | ≤0.09 |
| 105 DEG C of volatile matter % | ≤0.5 | ≤0.5 |
| Water extract resistivity Ω M | ≥30 | |
| Colour system system lightness l value | ≥98.4 | |
| Water dispersible % | ≥65 |
Although embodiment of the present invention are open as above, but it is not restricted to listed in specification sheets and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend described.
Claims (8)
1. the bleaching method of metatitanic acid in Titanium White Production By Sulfuric Acid Process, is characterized in that, comprise the following steps:
Step one, will containing Fe
3+impurity add in reactor through washing qualified metatitanic acid, add water after stirring, then add industrial sulphuric acid;
Step 2, EDTA-2Na is added in the metatitanic acid slurry of step one, keep temperature in reactor between 40 ~ 45 DEG C;
Step 3, the metatitanic acid slurry cooling that step 2 is obtained, vacuum filtration, washing;
Wherein, in described step 2, by EDTA-2Na:Fe
3+add in the metatitanic acid slurry of step one with mol ratio 2 ~ 4:1 gradation under whipped state.
2. the bleaching method of metatitanic acid in Titanium White Production By Sulfuric Acid Process as claimed in claim 1, is characterized in that, in described step 2, continue heating and makes the temperature in reactor be incubated 1 ~ 1.5h at 40 ~ 45 DEG C.
3. the bleaching method of metatitanic acid in Titanium White Production By Sulfuric Acid Process as claimed in claim 1, is characterized in that, add industrial sulphuric acid and make the sulfuric acid concentration of metatitanic acid slurry between 35 ~ 45g/L in described step one.
4. the bleaching method of metatitanic acid in Titanium White Production By Sulfuric Acid Process as claimed in claim 3, is characterized in that, in described step one in metatitanic acid slurry containing TiO
2between 235 ~ 245g/L.
5. the bleaching method of metatitanic acid in Titanium White Production By Sulfuric Acid Process as claimed in claim 4, is characterized in that, in described step one, pass into and be steam heated to 40 ~ 45 DEG C in reactor.
6. the bleaching method of metatitanic acid in Titanium White Production By Sulfuric Acid Process as claimed in claim 1, is characterized in that, in described step 3 with water coolant by metatitanic acid slurry cool to room temperature.
7. the bleaching method of metatitanic acid in Titanium White Production By Sulfuric Acid Process as claimed in claim 6, is characterized in that, filter metatitanic acid slurry in described step 3 by the leaf filter midge with negative pressure of vacuum.
8. the bleaching method of metatitanic acid in Titanium White Production By Sulfuric Acid Process as claimed in claim 7, is characterized in that, wash metatitanic acid in described step 3 with sand filter water.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104477985A (en) * | 2014-12-04 | 2015-04-01 | 攀钢集团钛业有限责任公司 | Bleaching method used in production of titanium dioxide powder by sulfuric acid process |
| CN106673059A (en) * | 2015-11-05 | 2017-05-17 | 四川航都钛业科技有限公司 | Process for bleaching metatitanic acid by using sodium citrate method |
| CN107986325B (en) * | 2017-10-16 | 2019-12-06 | 河北麦森钛白粉有限公司 | method for removing Fe2O3 from metatitanic acid in titanium dioxide as decorative base paper by sulfuric acid process |
| CN109607604B (en) * | 2018-12-14 | 2021-09-14 | 攀枝花东方钛业有限公司 | Metatitanic acid bleaching system and method |
| CN114014355B (en) * | 2021-09-16 | 2023-07-25 | 攀枝花学院 | Industrial meta-titanic acid purifying and deironing method |
| CN113818037A (en) * | 2021-09-16 | 2021-12-21 | 山东晟融泰新材料科技有限责任公司 | Electrolysis device for electrolyzing trivalent titanium from titanium white by sulfuric acid process |
| CN113697854A (en) * | 2021-09-16 | 2021-11-26 | 山东晟融泰新材料科技有限责任公司 | Process for electrolyzing trivalent titanium from titanium white by sulfuric acid method |
| CN113929132A (en) * | 2021-09-24 | 2022-01-14 | 东华工程科技股份有限公司 | Sulfuric acid method titanium dioxide metatitanic acid bleaching method and system |
| CN113845144A (en) * | 2021-09-30 | 2021-12-28 | 中国有色集团（广西）平桂飞碟股份有限公司 | Harmless resource utilization method for titanium dioxide acidolysis waste by sulfuric acid process |
| CN114671460B (en) * | 2022-04-27 | 2024-01-16 | 攀枝花学院 | Method for removing impurities from industrial meta-titanic acid in sulfuric acid method titanium dioxide short-process technology |
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