CN107814413B - The preparation method of water nano titanium oxide sol - Google Patents
The preparation method of water nano titanium oxide sol Download PDFInfo
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- CN107814413B CN107814413B CN201711104311.2A CN201711104311A CN107814413B CN 107814413 B CN107814413 B CN 107814413B CN 201711104311 A CN201711104311 A CN 201711104311A CN 107814413 B CN107814413 B CN 107814413B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
Abstract
The invention discloses the synthetic methods of a kind of nanometer of titanium oxide sol, the described method comprises the following steps: (1) acidolysis；(2) titanium liquid purifies；(3) sulfate radical removes；(4) it is catalytically decomposed；(5) it is centrifugated.Preparation method according to the present invention uses cheap ilmenite for raw material, without obtaining positive metatitanic acid by alkali precipitation titanyl sulfate, this method uses barium peroxide as reactive material, directly sulfate ion is precipitated, peroxide root and titanium ion are formed into complex simultaneously and are dissolved in water, reaction condition is mild, and step is easy；Meanwhile by introducing Fe3O4As Fenton catalyst, avoid the gelation of titanium peroxide and the heterogeneous nucleation process on barium sulfate surface, the titanium oxides product granule-morphology of preparation is uniform, can largely save the use of alkali and the discharge of waste water, and preparation method according to the present invention simple process is suitble to large-scale industrial production.
Description
Technical field
The invention belongs to inorganic titanium oxide preparation fields, in particular to high-activity nano TiO2The preparation side of sol material
Method.
Background technique
Titanium dioxide is important Inorganic Chemicals, in coating, ink, papermaking, plastics, rubber, the works such as synthetic fibers
It is used as white pigment in industry；Meanwhile in enamel, ceramics, welding rod, electronics, metallurgy etc. is industrial also important application.
Generally there are two kinds of technique productions of sulfuric acid process and chloridising: traditional sulfuric acid process industrial production titanium white powder flow path
Long, three waste discharge is more, and obtained product particle is big and uneven, is difficult to control；And chloridising is to ingredient requirement height, equipment corrosion
Seriously, preparation condition is harsh.
TiO 2 sol is with a wide range of applications as the uniform and stable dispersion of nano-titanium dioxide, can be with
For the synthesis of photocatalytic film coating or automatically cleaning high grade paint etc..Currently, preparing TiO 2 sol generally uses titanium
The method of organic compound control hydrolysis or Ti-inorganic salt hydrolysis.Utilize the method preparation two of titanium organic compound control hydrolysis
TiOx nano colloidal sol greatly improves cost since titanium organic compound is expensive；Simultaneously as mixed using alcohol water
Heshui solution, obtained product are organic solution, limit it and apply in hydrophilic base.Using Ti-inorganic salt hydrolysis, height is needed
The additional steps such as warm water thermal crystallisation, not only need special installation and device, increase cost, also limit production scale.
As the compound anion method for preparing rutile type titanium dioxide method patent of number of patent application 91101522.1 is also reported
The titanium sulfate solution obtained using sulfuric acid decomposition ilmenite is added composite anion and prepares rutile titanium dioxide, but it is needed
The high temperature crystallization process for wanting subsequent 800-900 DEG C this not only adds apparatus and process difficulty and improves cost, while also due to
High temperature sintering causes powder reuniting to increase partial size.Hiroaki Katsuki[Journal of the Ceramic Society
Of Japan 106 [3] 344~347 1998] it reports and dissolves the positive metatitanic acid obtained by titanium tetrachloride hydrolysis using hydrogen peroxide
The method that precipitating prepares TiO 2 sol.Since it uses corrosivity titanium tetrachloride for presoma, the high requirements on the equipment, thus
Industrial production cost is excessively high.
Summary of the invention
In view of the above-mentioned problems of the prior art, it is an object of the present invention to preparing Detitanium-ore-type in sulfuric acid process
On the basis of the conventional method of titanium dioxide, provide using ilmenite as the synthetic method of the nanometer titanium oxide sol of raw material, it is real
Existing normal pressure, low temperature liquid phase synthesize nanometer titanium oxide, can significantly reduce reaction process and production cost.
The synthetic method of nanometer titanium oxide sol according to the present invention the following steps are included:
(1) acidolysis
Ilmenite, the ilmenite and the concentrated sulfuric acid are dissolved by heating with the concentrated sulfuric acid that weight percent concentration is 80wt% or more
Mass ratio be 1:0.5 to 1:6, react fierce and generally completed in 5~30min rapidly, react maximum temperature up to 250 DEG C, obtain
To solid precipitation object obtain titanium liquid with the water extraction of 5-10 times of volume；
(2) titanium liquid purifies
The titanium liquid of step (1) is filtered and removes insoluble slag, frozen recrystallization is obtained with being filtered to remove ferrous sulfate
To the precursor solution of titaniferous；
(3) sulfate radical removes
The precursor solution in step 2) is diluted with water to sulfur acid oxygen titanium (TiOSO4) mass percent is
The solution of 5wt% to 20wt%, by BaO2Being dispersed in water and forming mass percent concentration is 5wt% to 20wt%, preferably
The BaO of 10wt%2Suspension, then according to the ratio that Ti:Ba molar ratio is 1:0.2 to 1:8 by BaO2Suspension is added to dilution
In the precursor solution of titaniferous afterwards, orange-yellow emulsion is obtained；
(4) it is catalytically decomposed
Fe is added into orange-yellow emulsion obtained in step 3)3O4Powder is to Fe3O4Molar concentration be 0.005 to
0.1mol/l, 90-100 DEG C of reflux 30min, obtain light yellow emulsion.
(5) it is centrifugated
Light yellow emulsion obtained in step 4) is utilized into centrifuge precipitation and separation and supernatant, it is obtained orange-yellow
Clear is titanium oxides product colloidal sol.
Preferably, in step 1), the mass ratio of the ilmenite and the concentrated sulfuric acid is 1:0.5 to 1:4, and more preferably 1:1 is extremely
1:3, most preferably 1:2.
Preferably, in step 1), the obtained solid precipitation object obtains titanium liquid with the water extraction of 6-8 times of volume, more excellent
It is selected as the water of 7.5 times of volumes.
Preferably, in step 3), the Ti:Ba molar ratio be 1:0.5 to 1:4, more preferably 1:0.6 to 1:2, most preferably
For 1:1 to 1:1.2.
Preferably, in step 3), the precursor solution in step 2) is diluted with water to sulfur acid oxygen titanium
(TiOSO4) solution of the mass percent for 5wt% to 15wt%, more preferably 10wt%.
Preferably, in step 4), Fe is added into orange-yellow emulsion obtained in step 3)3O4Powder is to Fe3O4Rub
Your concentration is 0.005 to 0.06mol/l, more preferably 0.005 to 0.02mol/l, most preferably 0.01mol/l.
Preferably, preparation method according to the present invention carries out as follows:
1) concentrated sulfuric acid that mass percent concentration is 80wt% or more is dissolved by heating into ilmenite, wherein ilmenite and sulfuric acid
Mass ratio be 1:2, obtained solid precipitation object obtains titanium liquid with the water extraction of 7.5 times of volumes, is then filtered to remove insoluble
Slag；
2) the titanium liquid frozen recrystallization in step 1) is obtained into the precursor solution of titaniferous to be filtered to remove ferrous sulfate；
3) precursor solution in step 2) is diluted to sulfur acid oxygen titanium (TiOSO4) mass percent is
The solution of 10wt%；Taking mass percent described in 200g is that 10wt% titanyl sulfate solution addition 250g mass percent is
The BaO of 10wt%2Suspension, wherein the molar ratio of Ti:Ba is about 1:1.2；
4) Fe of 1g is added into mixture obtained in step 3)3O4Powder, the 30min that flows back at 100 DEG C obtain yellow
Colloidal sol；
5) yellow sol obtained in step 4) is centrifugally separating to obtain clear titanyl with centrifuge 5000rpm
Compound product colloidal sol.
It is another object of the present invention to provide a kind of titanium oxides product aerosol product, the titanium oxides product is molten
Glue product is prepared by preparation method according to the present invention.
Beneficial effect
Preparation method according to the present invention uses cheap ilmenite for raw material, avoids using expensive organic metatitanic acid
Ester type compound, while without by alkali precipitation titanyl sulfate obtaining positive metatitanic acid, then multiple washing removing sulfate ion,
Alkaline precipitating agent obtains pure positive metatitanic acid, then nano-titanium oxide is prepared with hydrogen peroxide dissolution.This method peroxidating
Barium directly precipitates sulfate ion as reactive material, while peroxide root and titanium ion are formed complex and are dissolved in water, reacts
Mild condition, step are easy；Meanwhile by introducing Fe3O4As Fenton catalyst, avoid titanium peroxide gelation and
The titanium oxides product granule-morphology of the heterogeneous nucleation process on barium sulfate surface, preparation is uniform, can largely save alkali use and
The discharge of waste water, preparation method according to the present invention simple process are suitble to large-scale industrial production.
Detailed description of the invention
Fig. 1 is the TEM figure of product prepared by embodiment 1；
Fig. 2 is product XRD spectra prepared by embodiment 1；
Fig. 3 is that the methylene blue of product prepared by embodiment 1 decomposes ultraviolet spectrogram.
Specific embodiment
Hereinafter, will be described in detail the present invention.Before doing so, it should be appreciated that in this specification and appended
Claims used in term should not be construed as being limited to general sense and dictionary meanings, and inventor should allowed
On the basis of the appropriate principle for defining term to carry out best interpretations, according to meaning corresponding with technical aspect of the invention and generally
Thought explains.Therefore, description presented herein is not intended to limitation originally merely for the sake of the preferred embodiment for illustrating purpose
The range of invention, it will thus be appreciated that without departing from the spirit and scope of the present invention, it can be obtained by it
His equivalents or improved procedure.
General synthetic method obtains titanyl sulfate as precursor synthesis nano-titanium oxide by sulfuric acid process acidolysis, needs to use
Alkali precipitation obtains positive metatitanic acid, then removes sulfate ion, alkaline precipitating agent in multiple washing, obtains pure positive metatitanic acid, then
Nano-titanium oxide is prepared with hydrogen peroxide dissolution.This method directly uses barium peroxide as reactive material, directly by sulfuric acid
Radical ion precipitating, while peroxide root and titanium ion are formed into complex and are dissolved in water, sulfuric acid can be realized by simple centrifugally operated
Barium separation and titanium peroxide precursor preparation.Simultaneously as there are serious polycondensation reaction, above-mentioned barium sulfate peroxidating for titanium peroxide
Titanium system is directly centrifuged operation and will lead to form gel；And above-mentioned barium sulfate titanium peroxide system directly heats reaction
Titanium oxide precipitate can be made to grow on barium sulfate precipitate surface, be unable to get high-purity titanium oxide sol.The present invention passes through to titanium oxide
The mechanism regulation of liquid growth, the method for realizing normal pressure, low temperature liquid phase synthesis related system oxide material.Pass of the invention
Key point is using barium peroxide while generating through precipitating removing sulfate ion；And it introduces peroxide and forms titanium mistake with ion
Oxygen complex, while titanium oxide is obtained using the fenton principle of Fe catalysis fast decoupled peroxide root.By introducing Fe3O4Make
For catalyst, is decomposed based on Fenton mechanism quick catalysis titanium peroxide, form stable titanium oxide sol system and barium sulfate
Suspension system realizes that separation barium sulfate precipitate obtains high-purity titanium oxide sol by centrifugation.The present invention can be used for being directly realized by
Normal pressure, low temperature liquid phase synthesize nanometer titanium oxide, can significantly reduce reaction process and production cost.
The synthetic method of nanometer titanium oxide sol according to the present invention the following steps are included:
(1) acidolysis
Ilmenite, the ilmenite and the concentrated sulfuric acid are dissolved by heating with the concentrated sulfuric acid that weight percent concentration is 80wt% or more
Mass ratio be 1:0.5 to 1:6, react fierce and generally completed in 5~30min rapidly, react maximum temperature up to 250 DEG C, obtain
To solid precipitation object obtain titanium liquid with the water extraction of 5-10 times of volume；
(2) titanium liquid purifies
The titanium liquid of step (1) is filtered and removes insoluble slag, frozen recrystallization is obtained with being filtered to remove ferrous sulfate
To the precursor solution of titaniferous；
(3) sulfate radical removes
The precursor solution in step 2) is diluted with water to sulfur acid oxygen titanium (TiOSO4) mass percent is
The solution of 5wt% to 20wt%, by BaO2Being dispersed in water and forming mass percent concentration is 5wt% to 20wt%, preferably
The BaO of 10wt%2Suspension, then according to the ratio that Ti:Ba molar ratio is 1:0.2 to 1:8 by BaO2Suspension is added to dilution
In the precursor solution of titaniferous afterwards, orange-yellow emulsion is obtained；
(4) it is catalytically decomposed
Fe is added into orange-yellow emulsion obtained in step 3)3O4Powder is to Fe3O4Molar concentration be 0.005 to
0.1mol/l, 90-100 DEG C of reflux 30min, obtain light yellow emulsion.
(5) it is centrifugated
Light yellow emulsion obtained in step 4) is utilized into centrifuge precipitation and separation and supernatant, it is obtained orange-yellow
Clear is titanium oxides product colloidal sol.
Wherein in step 1), the mass ratio of the ilmenite and the concentrated sulfuric acid is 1:0.5 to 1:4, more preferably 1:1 to 1:3,
Most preferably 1:2.When the mass ratio of ilmenite and the concentrated sulfuric acid is greater than 1:1, i.e., the amount of ilmenite is superfluous, then cannot give birth to completely
At TiOSO4, a large amount of ilmenite raw materials are contained in titanium liquid, becomes impurity, causes to be difficult in second step through frozen recrystallization mistake
Filter out ferrous sulfate；When the mass ratio of ilmenite and the concentrated sulfuric acid is less than 1:3, i.e. excess sulfuric acid then not only generates
TiOSO4, but also generate Ti (SO4)2, the waste of titanium source is caused, while being difficult to control the content of titanium in titanium liquid, and then be difficult to control
Later period BaO processed2With the ratio of titanium.
Preferably, in step 1), the obtained solid precipitation object obtains titanium liquid with the water extraction of 6-8 times of volume, more excellent
It is selected as the water of 7.5 times of volumes.If less than the 6 times volumes of water used, leaching is incomplete；And if it is greater than 8 times of volumes, then titanium
The problems such as liquid concentration is too low, causes late phase reaction rate degradation.
Preparation method according to the present invention, the molar ratio of Ti:Ba are one of keys, it is preferable that in step 3), the Ti:
Ba molar ratio is 1:0.5 to 1:4, more preferably 1:0.6 to 1:2, most preferably 1:1 to 1:1.2.When Ti:Ba molar ratio is greater than
1:0.6, i.e. ti excess, then titanium peroxide is easy to happen polycondensation reaction, forms gel flocculation with barium sulfate, it is difficult to be centrifugated；
When Ti:Ba molar ratio is less than 1:2, i.e. barium is excessive, then equally be easy to cause titanium peroxide that polycondensation reaction occurs.
Preferably, in step 4), Fe is added into orange-yellow emulsion obtained in step 3)3O4Powder is to Fe3O4Rub
Your concentration is 0.005 to 0.06mol/l, more preferably 0.005 to 0.02mol/l, most preferably 0.01mol/l.Work as Fe3O4's
When molar concentration is less than 0.005mol/l, then titanium peroxide can not be made to decompose completely, stable titanium oxide sol body cannot be formed
System and barium sulfate suspension system；When being greater than 0.02mol/l, then titanium peroxide decomposition rate is too fast, is difficult to control, causes oxygen
Change titanium colloidal sol and barium sulfate particle flocculates.
Following embodiment is enumerated only as the example of embodiment of the present invention, does not constitute any limit to the present invention
System, it will be appreciated by those skilled in the art that modification in the range of without departing from essence and design of the invention each falls within the present invention
Protection scope.Unless stated otherwise, reagent and instrument used in the following embodiment are commercially available product.
Embodiment 1
1) concentrated sulfuric acid that mass percent concentration is 85wt% is dissolved by heating into ilmenite, wherein the matter of ilmenite and sulfuric acid
Amount is than for 1:2, obtained solid precipitation object obtains titanium liquid with the water extraction of 7.5 times of volumes, is then filtered to remove insoluble slag；
2) the titanium liquid frozen recrystallization in step 1) is obtained into the precursor solution of titaniferous to be filtered to remove ferrous sulfate；
3) precursor solution in step 2) is diluted to sulfur acid oxygen titanium (TiOSO4) mass percent is
The solution of 10wt%；Taking mass percent described in 200g is that 10wt% titanyl sulfate solution addition 250g mass percent is
The BaO of 10wt%2Suspension, wherein the molar ratio of Ti:Ba is about 1:1.2；
4) Fe of 1g is added into mixture obtained in step 3)3O4Powder, the 30min that flows back at 100 DEG C obtain yellow
Colloidal sol；
5) yellow sol obtained in step 4) is centrifugally separating to obtain clear titanyl with centrifuge 5000rpm
Compound product colloidal sol.
Product result is characterized as nano particle through TEM, sees attached drawing 1.Obtained titanium oxides product colloidal sol is dry by vacuum
Nano-titanium dioxide powder is obtained after dry, XRD spectra measurement result is confirmed that it is anatase titanium dioxide crystal, sees attached drawing 2.
Embodiment 2
Other than the mass ratio of ilmenite and the concentrated sulfuric acid is 1:3, titanium oxide is prepared according to the identical mode of embodiment 1
Product colloidal sol.
Embodiment 3
Other than the molar ratio of Ti:Ba in step 3) is adjusted to 1:0.6, titanium is prepared according to the identical mode of embodiment 1
Oxide products colloidal sol.
Embodiment 4
In addition to Fe in step 4)3O4Molar concentration be adjusted to other than 0.02mol/l, according to the identical mode system of embodiment 1
Standby titanium oxides product colloidal sol.
Comparative example 1
Other than the molar ratio of Ti:Ba in step 3) is adjusted to 1:4, titanyl is prepared according to the identical mode of embodiment 1
Compound product colloidal sol, but can not effectively obtain titanium oxides product colloidal sol.
Comparative example 2
In addition to Fe in step 4)3O4Molar concentration be adjusted to other than 0.06mol/l, according to the identical mode system of embodiment 1
Standby titanium oxides product colloidal sol, but titanium peroxide decomposition rate is too fast, and titanium oxide mutually flocculates with barium sulfate particle, generates a large amount of
Precipitating, is unable to get titanium oxides product colloidal sol.
Comparative example 3
Other than the molar ratio of Ti:Ba in step 3) is adjusted to 1:0.5, titanium is prepared according to the identical mode of embodiment 1
Oxide products colloidal sol, but can not effectively obtain titanium oxides product colloidal sol.
Comparative example 4
In addition to Fe in step 4)3O4Molar concentration be adjusted to other than 0.005mol/l, according to the identical mode of embodiment 1
Titanium oxides product colloidal sol is prepared, stable titanium oxide sol system and barium sulfate suspension system cannot be formed.
EXPERIMENTAL EXAMPLE 1
The titanium oxides product colloidal sol prepared in embodiment 1 to 4 is formed a film by czochralski method in glass surface, 1* is intercepted
2cm width is immersed in the 1mmol methylene blue solution that 20ml after 24 hours, is immersed in 2mmol methylene blue solution, in 365nm
It is measured under ultraviolet irradiation condition to methylene blue degradation effect.The discomposing effect of embodiment 1 is shown in attached drawing 3, methylene blue degradation
Light requirement shines 62 minutes when rate is 50%；The product light requirement of embodiment 2 shines 61 minutes when methylene blue degradation rate is 50%；Methylene
The product light requirement of embodiment 2 shines 63 minutes when blue degradation rate is 50%；The product of embodiment 4 when methylene blue degradation rate is 50%
Light requirement shines 64 minutes.It can be seen that the titanium oxides product colloidal sol of preparation according to the present invention can effectively realize organic matter etc.
Degradation, have broad application prospects.
Claims (1)
1. the preparation method of a kind of nanometer of titanium oxide sol, which is characterized in that the preparation method carries out as follows:
1) concentrated sulfuric acid that mass percent concentration is 80wt% or more is dissolved by heating into ilmenite, wherein the matter of ilmenite and sulfuric acid
Amount is than for 1:2, obtained solid precipitation object obtains titanium liquid with the water extraction of 7.5 times of volumes, is then filtered to remove insoluble slag；
2) the titanium liquid frozen recrystallization in step 1) is obtained into the precursor solution of titaniferous to be filtered to remove ferrous sulfate；
3) precursor solution in step 2) is diluted to sulfur acid oxygen titanium (TiOSO4) mass percent be 10wt% it is molten
Liquid；Taking mass percent described in 200g is the BaO that 10wt% titanyl sulfate solution is added that 250g mass percent is 10wt%2It is outstanding
Turbid, wherein the molar ratio of Ti:Ba is about 1:1.2；
4) Fe of 1g is added into mixture obtained in step 3)3O4Powder, it is molten that the 30min that flows back at 100 DEG C obtains yellow
Glue；
5) yellow sol obtained in step 4) is centrifugally separating to obtain clear titanium oxide with centrifuge 5000rpm
Product colloidal sol.
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