CN107814411A - The preparation method of trivalent titanium solution - Google Patents
The preparation method of trivalent titanium solution Download PDFInfo
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- CN107814411A CN107814411A CN201711209889.4A CN201711209889A CN107814411A CN 107814411 A CN107814411 A CN 107814411A CN 201711209889 A CN201711209889 A CN 201711209889A CN 107814411 A CN107814411 A CN 107814411A
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- C01G23/008—Titanium- and titanyl sulfate
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Abstract
The present invention relates to a kind of titanium white production technique, specifically discloses a kind of preparation method of trivalent titanium solution, comprises the following steps：A, in pressure vessel, one washes metatitanic acid slurry (by TiO2Count) (press H with the concentrated sulfuric acid2SO4Meter) mass ratio be 1:1.8~5 mixing；B, the concentration of sulfuric acid solution is determined；C, pressure vessel inside is pressurizeed according to the concentration of measure so that the boiling point of sulfuric acid solution is not less than 140 DEG C inside pressure vessel；D, heating and protect boiling at least 30min；E, stop heating, pressure release, cooling, add water to adjust concentration, add aluminium powder and the titanic in solution is reduced into titanous, that is, obtain trivalent titanium solution.It is an advantage of the invention that：Solve the stacking and pollution problem of titanium gypsum, and the production cost of trivalent titanium solution can be significantly reduced.
Description
Technical field
The present invention relates to a kind of titanium white production technique, especially a kind of sulfuric acid method titanium pigment production technology.
Background technology
Titanium dioxide is a kind of important Inorganic Chemicals, nontoxic, be harmless to the health, and is most important Chinese white,
The 80% of whole Chinese white usage amounts is accounted for, is widely used in coating, plastics, papermaking, printing-ink, chemical fibre, rubber, cosmetic
The industries such as product, food.The current titanium white production total amount in China up to 1,800,000 tons, titanium white production technique mainly have sulfuric acid process and
Two kinds of chloridising, China's production technology is based on sulfuric acid process.Its typical production process flow can be summarized as follows：
(1) acidolysis reaction is carried out with sulfuric acid with ilmenite concentrate or acid-dissolved titanium slag, obtains titanyl sulfate solution；
(2) hydrolysing titanyl sulfate solution obtains thick metatitanic acid slurry；
(3) thick metatitanic acid slurry is washed, salt treatment, obtains pretreatment metatitanic acid；
(4) pre-process metatitanic acid and be sent into rotary kiln calcining output TiO2Product.
Wherein, the technique washed to thick metatitanic acid slurry is specially：
(1) once wash：Separation of solid and liquid is carried out to thick metatitanic acid slurry, obtains a filter cake；Water-filling is entered to a filter cake
Wash to remove wherein iron ion, obtain one and wash metatitanic acid cake；One, which washes metatitanic acid cake, adds water to be beaten, and obtains one and washes metatitanic acid slurry；
(2) bleaching reduction：Addition bleaching agent and reducing agent in metatitanic acid slurry are washed toward one to be bleached, and it is brilliant to add calcining
Kind, obtain bleaching slurry；
(3) secondary washing：Separation of solid and liquid is carried out to bleaching slurry, obtains secondary filter cake；Secondary filter cake is washed with
Wherein iron ion is further removed, two is obtained and washes metatitanic acid cake；Two, which wash metatitanic acid cake, adds water to be beaten, and obtains two and washes metatitanic acid material
Slurry.
In sulfuric acid method titanium pigment production process, iron tramp the prolonging with washing time in metatitanic acid after once washing
Long, acidity reduces, and is gradually oxidized, and exists in the form of solid high ferro, can not be removed, has been converted to by washing
Fe/TiO2Ratio in 500~1000ppm or so.Trace Iron in metatitanic acid generates three oxygen of red after high-temperature calcination
Change two iron, be mixed into rutile lattice, cause lattice deformability, produce lattice defect, form chromophoric activity point so that product whiteness and
Reducing power declines, and has influence on the optical property of titanium dioxide, makes product rutile titanium white powder that yellow be presented.Therefore production rutile titanium
During white powder, it is necessary to washed away to once washing after metatitanic acid carries out bleaching reduction, then by secondary water except being mixed in metatitanic acid
Impurity iron.Method general at present is bleached using sulfuric acid, is then reduced using trivalent tiron, after secondary washing
Fe/TiO can be made20~30ppm is reduced to, the whiteness for obtaining finished product titanium dioxide significantly improves.
Trivalent tiron for reduction is commonly referred to as trivalent titanium solution, and its production method is to use to retrodeviate through once washing
It is prepared by metatitanic acid slurry：One is added in titanous preparation tank and washes metatitanic acid slurry, the concentrated sulfuric acid (often using 98 acid), heating acid is molten,
Then cool, add the desalted water regulation concentration of metering, the titanic in system is then reduced into titanous using aluminium powder, i.e.,
Obtain trivalent titanium solution.Production practices show that production ton trivalent titanium solution is (with TiO2Meter) 98 about 5~10 tons of acid need to be added.
Obtained trivalent titanium solution is used to bleach reduction process, and enters secondary washing step with technique, through secondary washing
Afterwards, caused waste water discharges after being handled into sewerage.Generally our waste water to discharge are neutralized using lime
Processing, neutralized reaction product is mainly titanium gypsum, and production ton titanium dioxide about consumes 0.04 ton of lime, and produces 0.2 ton of titanium gypsum, these
By-product titanium gypsum economic value is very low and needs to take substantial amounts of place stockpiling, and this is many sulfuric acid method titanium pigment production enterprises of puzzlement
One big problem of industry.
The content of the invention
To solve the occupation of land and pollution problem of titanium gypsum, the invention provides a kind of preparation method of trivalent titanium solution.
The technical solution adopted in the present invention is：The preparation method of trivalent titanium solution, comprises the following steps：
A, take one to wash metatitanic acid slurry to be well mixed with metering concentrated sulfuric acid injection pressure vessel, obtain mixture, it is described
The liquid phase of mixture is sulfuric acid solution；Described one washes metatitanic acid slurry (by TiO2Count) (press H with the concentrated sulfuric acid2SO4Meter) quality it
Than for 1:1.8~5；
B, determine and record the concentration of the sulfuric acid solution；
C, and then closed pressure container, and pressure vessel inside is pressurizeed according to the sulfuric acid solution concentration of measure, added
Pressure standard is so that the boiling point of sulfuric acid solution is not less than 140 DEG C inside pressure vessel；
D, pressure vessel internal-response system is carried out being heated to seething with excitement, and protects boiling at least 30min, obtain sour solution；
E, stop heating, pressure release, cooling, the water regulation concentration of metering is added into above-mentioned sour solution, then adds meter
Titanic in solution is reduced into titanous by amount aluminium powder, that is, obtains trivalent titanium solution.
Inventor find, in actual production, the trivalent titanium solution of production unit yield, the addition of the raw material concentrated sulfuric acid with
One wash metatitanic acid slurry concentration (i.e. titanium concentration) it is relevant.Inventor proposes that we may add in production practices at present accordingly
Excessive sulfuric acid, its main cause are that the sour molten needs for washing metatitanic acid slurry reach higher temperature, and we are through experiment survey
Will at least be reached by obtaining by 140 DEG C.And the boiling point of reaction system is elevated with the increase of sulfuric acid concentration in system, therefore only
When sulfuric acid reaches finite concentration in system, the boiling point of solution can be only achieved a suitable sour solubility temperature for washing metatitanic acid slurry, from
And can fully dissolve and wash metatitanic acid slurry, therefore one wash metatitanic acid pulp density it is lower, it is necessary to add sulfuric acid amount more
It is more.Inventor thinks that the sulfuric acid addition at present during trivalent titanium solution is prepared is above being actually needed value accordingly
's.
Inventor's research thinks that a main component for washing metatitanic acid slurry is the polymer of titanium dioxide and tied containing part
Heshui, it is to be translated into titanyl sulfate or the form of titanium sulfate is present that our conventional concentrated sulfuric acid dissolutions one, which wash metatitanic acid its essence,
In solution, according to this premise, if one washes metatitanic acid and is completely converted into titanyl sulfate, the required concentrated sulfuric acid (presses H2SO4Meter)
Quality should wash metatitanic acid slurry (by TiO2Meter) 1.2 times of quality；And if one washes metatitanic acid and is completely converted into titanium sulfate,
Then the required concentrated sulfuric acid (presses H2SO4Meter) quality should wash metatitanic acid slurry (by TiO2Meter) 2.4 times of quality.It is but molten
Dihydroxy complex of the titanyl sulfate its essence is titanium in aqueous in liquid, the material easily hydrolyze in the solution,
Titanium precipitation is formed, therefore in order to prevent the Substance P hydrolysis, the titanium in sour solution, which should try one's best in the form of titanium sulfate, to be present.
That is, the required concentrated sulfuric acid (presses H in theory2SO4Meter) quality should wash metatitanic acid slurry (by TiO2Meter) 2.4 times of quality.
Further it has been found that the dihydroxy complex that a small amount of titanium in sour solution be present is not allow
, because the precipitation reaction of titanyl sulfate is just occurred under certain acidity, temperature and time, and due to tetravalence titanium ion
External electrical be really after electronics on D2SP3 tracks all loses, orbital hybridization, form complex, its coordinationization
Compound contains two hydroxyls (being coordinated by lone electron) and four molecular waters, so being easy to that intermolecular dehydration occurs, it is heavy to be formed
Form sediment and react.So as to which in subsequent technique, titanous can be reduced into by the addition of aluminium powder, its essence is exist by electronics
Occupy-place is carried out on the coordination track of titanium ion, is reduced with the hydroxyl value for ion, therefore change (can for the stability of ion
The hydroxyl value for carrying out intermolecular dehydration is reduced), intermolecular formation titanium precipitation becomes difficult, so not being very high even in acidity, it is impossible to
Completely formed titanium sulfate in the case of, can also stablize preparation trivalent titanium solution.We conducted experimental study, experiment accordingly
Demonstrate, according to method of the invention when the concentrated sulfuric acid (presses H2SO4Meter) quality as little as one wash metatitanic acid slurry (by TiO2Meter) matter
Amount 1.8 times when still can stablize preparation trivalent titanium solution.
Yet with the present invention we greatly reduce the addition of the concentrated sulfuric acid, this will cause sulfuric acid concentration in solution
Substantially reduce, the boiling point of solution can not reach the molten required temperature of acid, therefore, it is proposed that reaction system can be placed in into pressure vessel
Middle carry out compressive reaction.Reach the purpose of lifting solution boiling point by the raising of reaction pressure.It can be managed according to analysis above
Solution, the pressure of pressure vessel should be adjusted according to the concentration of wherein sulfuric acid solution, sulfuric acid solution concentration it is lower, it is necessary to pressure
Qiang Yuegao.
We also demonstrate that in an experiment, quality can be added into pressure vessel is at least and wash metatitanic acid slurry and (press
TiO2Meter) 1.8 times of the concentrated sulfuric acid (presses H2SO4Meter), and by determining the sulfuric acid solution concentration before reacting, with by controlling pressure
Promote to wash the molten purpose of metatitanic acid slurry acid to reach.And when the concentrated sulfuric acid (presses H2SO4Meter) addition washes metatitanic acid material more than one
Slurry (presses TiO2Meter) 5 times of quality when, then only need by way of metatitanic acid pulp density and sulfuric acid concentration are washed in control one, adopt
The preparation of trivalent tiron is carried out with conventional method.
Corresponding boiling point can be determined the sulfuric acid solution of various concentrations by this area normal experiment at various pressures,
Following table is some experimental data that applicant provides：
Such as metatitanic acid slurry is washed (by TiO when one2Count) (press H with the concentrated sulfuric acid2SO4Meter) mass ratio press 1:1.8 ratio
Example adds, and one washes metatitanic acid pulp density by TiO2300g/L is calculated as, when the concentrated sulfuric acid is 98 sour, it is molten to measure sulfuric acid in step A
The mass concentration of liquid is about 10%, and now pressure vessel internal pressure is that 0.35MPa can ensure that sulfuric acid solution boiling point more than 140
℃。
Trivalent titanium solution enters sewage system after bleaching is washed in the form of titanic, residual titanous, free sulfuric acid etc.
System.
The beneficial effects of the invention are as follows：Due to the method by the present invention can reduction to the full extent to prepare titanous molten
The addition of the concentrated sulfuric acid during liquid, therefore in subsequent technique, enter secondary washing step with trivalent titanium solution, and through secondary
Caused free sulfuric acid greatly reduces after washing step, and the lime consumption that thus be accordingly used in neutralization waste water is greatly reduced, so as to raw
Into titanium gypsum be also accordingly greatly reduced, solve the stacking and pollution problem of titanium gypsum, and trivalent titanium solution can be significantly reduced
Production cost.
Embodiment
With reference to embodiment, the present invention is further described.
Embodiment one：
Trivalent titanium solution A is prepared in accordance with the following methods：
(1) one is taken to wash metatitanic acid slurry (TiO2=300g/l) it is well mixed with 98 acid injection pressure vessels, mixed
Compound, the liquid phase of the mixture is sulfuric acid solution；Described one washes metatitanic acid slurry (by TiO2Count) (press H with 98 acid2SO4Meter)
Mass ratio be 1:1.8；
(2) sulfuric acid solution mass concentration is measured as 9.9%；
(3) and then closed pressure container, pressurize and control pressure vessel internal pressure in 0.35Mpa；
(4) pressure vessel internal-response system is carried out being heated to seething with excitement, and protects boiling 30min, obtain the molten solution of acid；
(5) stop heating, pressure release, be cooled to 70 DEG C, added into above-mentioned sour solution metering water adjust concentration to
TiO2=90g/l, then add aluminium powder (mass values of aluminium powder and total titanium dioxide are 0.11) by the titanic in solution also
Original obtains trivalent titanium solution A into titanous.
(6) trivalent titanium solution A titanous concentration and clarity is detected, the results are shown in Table 1.
Embodiment two：
Trivalent titanium solution B is prepared in accordance with the following methods：
(1) one is taken to wash metatitanic acid slurry (TiO2=300g/l) it is well mixed with 98 acid injection pressure vessels, mixed
Compound, the liquid phase of the mixture is sulfuric acid solution；Described one washes metatitanic acid slurry (by TiO2Count) (press H with 98 acid2SO4Meter)
Mass ratio be 1:2.4；
(2) sulfuric acid solution mass concentration is measured as 12.3%；
(3) and then closed pressure container, pressurize and control pressure vessel internal pressure in 0.32Mpa；
(4) pressure vessel internal-response system is carried out being heated to seething with excitement, and protects boiling 40min, obtain the molten solution of acid；
(5) stop heating, pressure release, be cooled to 70 DEG C, added into above-mentioned sour solution metering water adjust concentration to
TiO2=90g/l, then add aluminium powder (mass values of aluminium powder and total titanium dioxide are 0.11) by the titanic in solution also
Original obtains trivalent titanium solution B into titanous.
(6) trivalent titanium solution B titanous concentration and clarity is detected, the results are shown in Table 1.
Embodiment three：
Trivalent titanium solution C is prepared in accordance with the following methods：
(1) one is taken to wash metatitanic acid slurry (TiO2=300g/l) with mass concentration be 93% the concentrated sulfuric acid inject pressure vessel
In be well mixed, obtain mixture, the liquid phase of the mixture is sulfuric acid solution；Described one washes metatitanic acid slurry (by TiO2Meter)
(H is pressed with the concentrated sulfuric acid2SO4Meter) mass ratio be 1:4.8；
(2) sulfuric acid solution mass concentration is measured as 47.2%；
(3) and then closed pressure container, pressurize and control pressure vessel internal pressure in 0.20Mpa；
(4) pressure vessel internal-response system is carried out being heated to seething with excitement, and protects boiling 40min, obtain the molten solution of acid；
(5) stop heating, pressure release, be cooled to 70 DEG C, added into above-mentioned sour solution metering water adjust concentration to
TiO2=90g/l, then add aluminium powder (mass values of aluminium powder and total titanium dioxide are 0.11) by the titanic in solution also
Original obtains trivalent titanium solution C into titanous.
(6) trivalent titanium solution C titanous concentration and clarity is detected, the results are shown in Table 1.
Example IV：
Trivalent titanium solution D is prepared in accordance with the following methods：
(1) one is taken to wash metatitanic acid slurry (TiO2=300g/l) it is well mixed with 98 acid injection titanous preparation tanks, obtain
Metatitanic acid slurry is washed (by TiO to mixture, described one2Count) (press H with 98 acid2SO4Meter) mass ratio be 1:5；
(2) it is heated to seething with excitement, and protects boiling 30min, obtains the molten solution of acid；
(3) stop heating, be cooled to 70 DEG C, the water that metering is added into above-mentioned sour solution adjusts concentration to TiO2=
90g/l, then add aluminium powder (mass values of aluminium powder and total titanium dioxide are 0.11) and the titanic in solution is reduced into three
Valency titanium, that is, obtain trivalent titanium solution D.
(4) trivalent titanium solution D titanous concentration and clarity is detected, the results are shown in Table 1.
Table 1：Trivalent titanium solution testing result table
| Clarity | Titanous concentration | Ton product sulfuric acid consumption | |
| Trivalent titanium solution A | Clarification | 90.3g/l | 1.8t |
| Trivalent titanium solution B | Clarification | 90.3g/l | 2.4t |
| Trivalent titanium solution C | Clarification | 90.4g/l | 4.8t |
| Trivalent titanium solution D | Clarification | 90.3g/l | 5.0t |
Claims (6)
1. the preparation method of trivalent titanium solution, comprises the following steps：
A, take one to wash metatitanic acid slurry to be well mixed with metering concentrated sulfuric acid injection pressure vessel, obtain mixture, the mixing
The liquid phase of thing is sulfuric acid solution；Described one washes metatitanic acid slurry (by TiO2Count) (press H with the concentrated sulfuric acid2SO4Meter) mass ratio be
1:1.8~5；
B, determine and record the concentration of the sulfuric acid solution；
C, and then closed pressure container, and pressure vessel inside is pressurizeed according to the sulfuric acid solution concentration of measure, pressurization mark
Standard is so that the boiling point of sulfuric acid solution is not less than 140 DEG C inside pressure vessel；
D, pressure vessel internal-response system is carried out being heated to seething with excitement, and protects boiling at least 30min, obtain sour solution；
E, stop heating, pressure release, cooling, the water regulation concentration of metering is added into above-mentioned sour solution, then adds metering aluminium
Titanic in solution is reduced into titanous by powder, that is, obtains trivalent titanium solution.
2. the preparation method of trivalent titanium solution according to claim 1, it is characterised in that：One washes inclined titanium described in step A
Sour slurry (presses TiO2Count) (press H with the concentrated sulfuric acid2SO4Meter) mass ratio be 1:1.8~2.4.
3. the preparation method of trivalent titanium solution according to claim 1, it is characterised in that：One washes inclined titanium described in step A
Sour slurry (presses TiO2Count) (press H with the concentrated sulfuric acid2SO4Meter) mass ratio be 1:2.4~5.
4. the preparation method of trivalent titanium solution according to claim 1, it is characterised in that：One washes inclined titanium described in step A
Sour slurry (presses TiO2Count) (press H with the concentrated sulfuric acid2SO4Meter) mass ratio be 1:1.8.
5. the preparation method of trivalent titanium solution according to claim 1, it is characterised in that：One washes inclined titanium described in step A
Sour slurry (presses TiO2Count) (press H with the concentrated sulfuric acid2SO4Meter) mass ratio be 1:2.4.
6. the preparation method of trivalent titanium solution according to claim 4, it is characterised in that：One washes inclined titanium described in step A
Sour pulp density presses TiO2300g/L is calculated as, the concentrated sulfuric acid is 98 acid, and pressure vessel internal pressure is 0.35MPa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111392767A (en) * | 2020-04-22 | 2020-07-10 | 龙佰四川钛业有限公司 | Method for preparing trivalent titanium by hydrolyzing scale |
| CN115367788A (en) * | 2022-07-11 | 2022-11-22 | 云南国钛金属股份有限公司 | Method for preparing trivalent titanium aqueous solution at low cost |
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| CN111392767A (en) * | 2020-04-22 | 2020-07-10 | 龙佰四川钛业有限公司 | Method for preparing trivalent titanium by hydrolyzing scale |
| CN115367788A (en) * | 2022-07-11 | 2022-11-22 | 云南国钛金属股份有限公司 | Method for preparing trivalent titanium aqueous solution at low cost |
| CN115367788B (en) * | 2022-07-11 | 2023-11-21 | 云南国钛金属股份有限公司 | Method for preparing trivalent titanium aqueous solution at low cost |
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Effective date of registration: 20210721 Address after: 543199 No. 15, Longcheng East Road, Longwei Town, Longwei District, Wuzhou City, Guangxi Zhuang Autonomous Region Patentee after: GUANGXI SHUNFENG TITANIUM INDUSTRY Co.,Ltd. Address before: 535011 12 Binhai Road, Binhai New Town, Qinzhou City, the Guangxi Zhuang Autonomous Region Patentee before: BEIBU GULF University |
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