CN103293044B - Dissolving method of high purity titanium dioxide - Google Patents
Dissolving method of high purity titanium dioxide Download PDFInfo
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- CN103293044B CN103293044B CN201310259538.XA CN201310259538A CN103293044B CN 103293044 B CN103293044 B CN 103293044B CN 201310259538 A CN201310259538 A CN 201310259538A CN 103293044 B CN103293044 B CN 103293044B
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Abstract
The invention provides a dissolving method for measuring the content of impurity elements suitable for high purity titanium dioxide. The dissolving method of high purity titanium dioxide comprises the following steps: 1) grinding high purity titanium dioxide, and drying and cooling; 2) weighing the high purity titanium dioxide obtained by the step 1), and placing the high purity titanium dioxide in a reaction tank; 3) adding hydrofluoric acid and hydrogen peroxide to heat, wherein the high purity titanium dioxide is completely dissolved; and 4) taking off a lid on the reaction tank, and adding concentrated sulfuric acid after distillation to continuously heat, wherein hydrofluoric acid in the liquor is volatilized; and cooling to complete. With the adoption of the dissolving method provided by the invention, the interference caused by introduced solvents is reduced to the maximum extent, the influence by interference signals is reduced, the analytic and detecting lower limit of elements to be detected is reduced, the sensitivity, accuracy and precision for analysis are improved, the analytical testing efficiency is greatly improved, and the analytical testing cost is low.
Description
Technical field
The present invention relates to a kind of dissolving method of high-purity titanium dioxide.
Background technology
The chemical property of high-purity titanium dioxide (purity > 99.9wt%) is very stable, under normal temperature hardly with other material generation chemical reaction, it is a kind of intermediate oxide of slant acidity, be slightly soluble in alkali and hot nitric acid, only could be dissolved in the concentrated sulphuric acid and hydrofluorite completely under long-time boiling conditions, therefore dissolution process be carried out to titania very difficult.The dissolving method of the high-purity titanium dioxide in usual laboratory is that high-purity titanium dioxide sample is placed in beaker, adds the concentrated sulphuric acid and ammonium sulfate solubilising reagent heating for dissolving on resistance furnace.Adopt this dissolving method length consuming time, sample dissolution amount is few, and add the how easy substitution impurity of reagent, toxic reagent volatility is large, to human body and environmental injury large, sulfuric acid concentration is comparatively large, and saliferous is higher, easily causes micro impurity element in high-purity titanium dioxide to analyze data distortion serious, accuracy and the precision of measurement result are poor, can not meet the requirement of the analysis of micro impurity element in high-purity titanium dioxide, therefore, above-mentioned dissolving method is unsuitable for the mensuration of the impurity content of high-purity titanium dioxide.
Summary of the invention
Technical matters to be solved by this invention is to provide the dissolving method that a kind of impurity content being suitable for high-purity titanium dioxide measures.
The technical scheme that technical solution problem of the present invention adopts is: the dissolving method of high-purity titanium dioxide, and the method comprises the following steps: after 1) being ground by high-purity titanium dioxide, cooling after dry; 2) step 1 is weighed) high-purity titanium dioxide that obtains, be positioned in retort; 3) heat after adding hydrofluorite and hydrogen peroxide, high-purity titanium dioxide is dissolved completely; 4) take off the lid in retort, add the concentrated sulphuric acid after distillation and continue heating, the hydrofluorite in solution is volatilized, has namely processed after cooling.
Further, between described high-purity titanium dioxide, hydrofluorite, hydrogen peroxide, the concentrated sulphuric acid, part by weight is: 0.9997 ~ 1.0003: 6.90 ~ 11.50: 0.32 ~ 0.64: 3.68 ~ 7.36.
Further, step 1) described drying puts into baking oven 105 ~ 115 DEG C of dryings 2 ~ 4 hours.
Further, step 1) described cooling is cooled to room temperature.
Further, step 3) described heating covers to be placed on electric boiling plate by the lid of retort to heat, electric boiling plate temperature controls at 220 ~ 260 DEG C, 40 ~ 50 minutes heat times.
Further, step 4) described distillation is that electric boiling plate temperature is risen to 300 ~ 350 DEG C, distills 10 ~ 20 minutes.
Further, step 4) described continue heating time be 10 ~ 20 minutes.
Further, described retort adopts polytetrafluoroethylstandard standard retort.
Further, step 3) purity >=40.0wt% of described hydrofluorite, the purity >=30.0wt% of described hydrogen peroxide.
Further, step 4) concentration >=98wt% of the described concentrated sulphuric acid.
The invention has the beneficial effects as follows: the inventive method dissolves high-purity titanium dioxide, and required quantity of solvent is less, impurity substitutes into few, and the amount of dissolving high-purity titanium dioxide is more, and dissolve required time completely short, be about 60 ~ 80 minutes, it is low that sample dissolves power consumption completely.Adopt dissolving method of the present invention, the interference caused because of the solvent of introducing can be reduced to greatest extent, reduce the impact of undesired signal, the analysis reducing element to be measured detects lower limit, improve sensitivity for analysis, accuracy and precision, very big raising analytical test efficiency, analytical test cost is low, operating process science is simple, safety, environmental protection.
Embodiment
Method of the present invention comprises the following steps:
1), after high-purity titanium dioxide being ground to granularity > 300 order, putting into baking oven and be cooled to room temperature 105 ~ 115 DEG C of dryings after 2 ~ 4 hours;
2) retort is put on balance weigh step 1) high-purity titanium dioxide that obtains, and it to be evenly positioned in retort;
3) in retort, add hydrofluorite, drip several hydrogen peroxide after the lid of retort covered to be placed on electric boiling plate heat, electric boiling plate temperature controls at 220 ~ 260 DEG C, and 40 ~ 50 minutes heat times, high-purity titanium dioxide is dissolved completely;
4) lid in retort is taken off, electric boiling plate temperature is risen to 300 ~ 350 DEG C, distill after 10 ~ 20 minutes and add concentrated sulphuric acid continuation heating 10 ~ 20 minutes, make hydrofluorite volatilization residual in solution, after cooling, solution is transferred to constant volume in volumetric flask, shakes up stand-by, high-purity titanium dioxide dissolution process completes.
Above-mentioned retort preferably adopts polytetrafluoroethylstandard standard retort, because this retort cost is far below platinum crucible, and because this retort is with interior plug, good leak tightness, solubilising reagent can be suppressed to volatilize, reduce solubilising reagent consumption largely, effectively shorten and dissolve high-purity titanium dioxide required time.
The purity of above-mentioned hydrofluorite is best >=40.0wt%, and the concentration of the above-mentioned concentrated sulphuric acid is best >=98wt%, and the purity of above-mentioned hydrogen peroxide is best >=30.0wt%.
Between above-mentioned high-purity titanium dioxide, hydrofluorite, hydrogen peroxide, the concentrated sulphuric acid, part by weight is preferably: 0.9997 ~ 1.0003: 6.90 ~ 11.50: 0.32 ~ 0.64: 3.68 ~ 7.36.
Embodiment:
1), after high-purity titanium dioxide being ground to granularity > 300 order, putting into 110 DEG C of baking ovens and be cooled to room temperature after dry 2 hours;
2) respectively the polytetrafluoroethylstandard standard retort (taking off the lid in retort) being numbered 1#, 2#, 3# is put on balance weigh step 1 respectively) the high-purity titanium dioxide 1.0000g that obtains, and it to be evenly positioned in polytetrafluoroethylstandard standard retort respectively;
3) in the polytetrafluoroethylstandard standard retort being numbered 1#, add with liquid-transfering gun the hydrogen peroxide (being converted into weight is 0.36g) that 8.0ml purity is 40.0wt% hydrofluorite (being converted into weight is 9.20g) and 5 purity are 30.0wt%; In the polytetrafluoroethylstandard standard retort being numbered 2#, the hydrogen peroxide (being converted into weight is 0.36g) that 8.0ml purity is 40.0wt% hydrofluorite (being converted into weight is 9.20g) and 5 purity are 30.0wt% is added with liquid-transfering gun; In the polytetrafluoroethylstandard standard retort being numbered 3#, the hydrogen peroxide (being converted into weight is 0.36g) that 8.0ml purity is 40.0wt% hydrofluorite (being converted into weight is 9.20g) and 5 purity are 30.0wt% is added with transfer pipet;
Be placed on electric boiling plate by above-mentioned 3 polytetrafluoroethylstandard standard retort cover lids and heat, electric boiling plate temperature controls at 240 DEG C, and till the high-purity titanium dioxide be heated in retort dissolves completely, the heat time is 40 ~ 50 minutes;
4) lid in above 3 retort is taken off, electric boiling plate temperature is risen to 350 DEG C, distill 10 minutes, adding 2ml (being converted into weight is 3.68g) concentration is that the concentrated sulphuric acid of 98wt% is in retort, heat 10 minutes again, after cooling, solution is transferred to constant volume in volumetric flask, shakes up stand-by, high-purity titanium dioxide dissolution process completes.
Dissolve solubilising reagent amount and dissolution process required time needed for high-purity titanium dioxide completely in table 1.
Table 1
As can be seen from the above table: when adopting the inventive method to dissolve 1.0000g high-purity titanium dioxide sample completely, hydrofluoric acid dissolution reagent consumption is 8.0ml (weight is 9.20g), concentrated sulphuric acid reagent consumption is 2ml (weight is 3.68g), and complete dissolution process required time is 60 ~ 75 minutes.By the inventive method, resolution process is carried out to high-purity titanium dioxide sample, the not volatile spilling of solubilising reagent (can reduce use amount and the discharge capacity of toxic chemical, effectively can reduce the pollution of chemical substance to environment), solubilising reagent consumption is few, and dissolution process sample required time is short, and energy consumption is little, analytical test is with low cost, operating process science, simple, safety, environmental protection, can greatly improve analytical test efficiency, this inventive method can extensively be used in the lab.
Claims (9)
1. the dissolving method of high-purity titanium dioxide, is characterized in that, the method comprises the following steps:
1) after high-purity titanium dioxide being ground, cooling after dry;
2) step 1 is weighed) high-purity titanium dioxide that obtains, be positioned in retort;
3) heat after adding hydrofluorite and hydrogen peroxide, high-purity titanium dioxide is dissolved completely, described heating-up temperature is 220 ~ 260 DEG C;
4) take off the lid in retort, add the concentrated sulphuric acid after distillation and continue heating, the hydrofluorite in solution is volatilized, has namely processed after cooling;
Between described high-purity titanium dioxide, hydrofluorite, hydrogen peroxide, the concentrated sulphuric acid, part by weight is: 0.9997 ~ 1.0003:6.90 ~ 11.50:0.32 ~ 0.64:3.68 ~ 7.36.
2. the dissolving method of high-purity titanium dioxide as claimed in claim 1, is characterized in that, step 1) described drying puts into baking oven 105 ~ 115 DEG C of dryings 2 ~ 4 hours.
3. the dissolving method of high-purity titanium dioxide as claimed in claim 1, is characterized in that, step 1) described cooling is cooled to room temperature.
4. the dissolving method of high-purity titanium dioxide as claimed in claim 1, it is characterized in that, step 3) described heating covers to be placed on electric boiling plate by the lid of retort to heat, electric boiling plate temperature controls at 220 ~ 260 DEG C, 40 ~ 50 minutes heat times.
5. the dissolving method of high-purity titanium dioxide as claimed in claim 1, is characterized in that, step 4) described distillation is that electric boiling plate temperature is risen to 300 ~ 350 DEG C, distills 10 ~ 20 minutes.
6. the dissolving method of high-purity titanium dioxide as claimed in claim 1, is characterized in that, step 4) the described time of continuing heating is 10 ~ 20 minutes.
7. the dissolving method of high-purity titanium dioxide as claimed in claim 1, is characterized in that, described retort adopts polytetrafluoroethylstandard standard retort.
8. the dissolving method of high-purity titanium dioxide as claimed in claim 1, is characterized in that, step 3) purity >=40.0wt% of described hydrofluorite, purity >=30.0% of described hydrogen peroxide.
9. the dissolving method of high-purity titanium dioxide as claimed in claim 1, is characterized in that, step 4) concentration >=98wt% of the described concentrated sulphuric acid.
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| CN103913431B (en) * | 2014-04-21 | 2016-10-26 | 济南裕兴化工有限责任公司 | The assay method of titanium dioxide acid solubility |
| CN104458369B (en) * | 2014-11-18 | 2017-08-29 | 湖北新华光信息材料有限公司 | A kind of preparation method of plasma spectroscopy detection titanium oxide solution sample |
| CN110420629A (en) * | 2019-07-25 | 2019-11-08 | 江苏申苏环境科技有限公司 | A kind of photocatalyst preparation method and applications of catalytic degradation formaldehyde |
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