CN106185832A - A kind of stably-doped peroxo titanic acid sol and preparation method thereof - Google Patents
A kind of stably-doped peroxo titanic acid sol and preparation method thereof Download PDFInfo
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- CN106185832A CN106185832A CN201610519414.4A CN201610519414A CN106185832A CN 106185832 A CN106185832 A CN 106185832A CN 201610519414 A CN201610519414 A CN 201610519414A CN 106185832 A CN106185832 A CN 106185832A
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- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/055—Peroxyhydrates; Peroxyacids or salts thereof
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Abstract
The present invention relates to a kind of stably-doped peroxo titanic acid sol and preparation method thereof, belong to chemical field.Preparation method of the present invention be the positive metatitanic acid that a kind of employing is prepared by industrial titanium sulphate solution be raw material, preparation stability is high, excellent performance, the method of stably-doped peroxo titanic acid sol: by the ratio of regulation and control stabilizer (alpha-hydroxy acid) with positive metatitanic acid, hydrogen peroxide and the ratio of positive metatitanic acid, system titanium concentration, regulation endpoint pH etc. prepares doping peroxo titanic acid sol.Colloidal sol doping can realize the uniform mixing on molecular level, and stability is high, and activity is high, and doping is flexibly.It is easy that the method has method, low cost, its lytic activity advantages of higher.A step doping poriferous titanium dioxide of anatase titanium dioxide crystal formation, bigger serface can be prepared according to the method that the present invention provides.
Description
Technical field
The present invention relates to a kind of stably-doped peroxo titanic acid sol and preparation method thereof, stable especially by adding
Agent, adjusts the consumption of stabilizer and with ammonia regulation pH to prepare stability height, the method for the doping pertitanic acid of excellent performance,
Belong to chemical field.
Technical background
Peroxo titanic acid sol is yellow or orange transparence, has stability high, good dispersion, and raw material is easy to get, it is not necessary to
Using expensive organic alkoxide, reaction system is neutrality, the advantages such as environmental pollution is less so that it is apply in system as presoma
Standby nano titanium oxide, TiO2Hollow ball, complex microsphere, low temperature catalyst, compound titanate and dye sensitization of solar electricity
In pond and flexible dye-sensitized solar battery.Have in titanio functional material, titanium-based film material, photocatalysis, environmental conservation etc.
There is the application prospect of broadness.It is little that this method has environmental pollution, and preparation technology, at low temperatures can be real simply without complex device
Existing TiO2The transformation of crystal formation, can be supported on above pottery, metal or low temperature organic substrate material and raw material sources are extensive, price is low
The advantage such as honest and clean.
The existing method preparing pertitanic acid is with expensive tetraethyl titanate, metatitanic acid isopropanol, metatitanic acid four mostly
The inorganic ti sources such as organic titanium source or analytically pure titanium tetrachloride, titanium sulfate such as butyl ester prepare titanic as the initial feed of synthesis
Acid carries out hydrogen peroxide peptization again, and the industrialization to be realized of these methods also needs to bigger improvement.And there is doping instability, easily
The shortcomings such as hydrolysis.Pure pertitanic acid stability is higher, but doping rear stability is substantially reduced, and is mainly in view of doping to peroxide
Change the impact of hydrogen.Hydrogen peroxide is more sensitive especially for transition metal ionss such as ferrum to part dopant ion, due to ferrum from
The concentration increase of son can cause the decomposition of hydrogen peroxide drastically to be accelerated so that the Complexation Efficiency of hydrogen peroxide with positive metatitanic acid significantly dropping
Low.Additionally, it is not in neutrality that doping often makes the pH of system, this also causes the stability of hydrogen peroxide to reduce, and accelerates
The decomposition of hydrogen oxide, ultimately results in the hydrolysis of pertitanic acid.
In the research of semiconductor nano photocatalyst, titanium dioxide has good energy gap, oxidability because of it
By force, nontoxic, the advantages such as biological, chemical and photochemical stability is good, are the current catalysis materials having most application potential, but dioxy
The photocatalysis performance changing titanium is mainly manifested under ultraviolet light, it is therefore necessary to it is doped modification, and doping can make it inhale
There is red shift in various degree and change its crystallite dimension in take-up so that it is the absorption band at visible ray increases, and improves its photocatalysis
Performance.During preparing the porous silica titanium precursors of bigger serface, load has the doping component of catalysis activity,
Reach a step and prepared advanced function material by industry primary raw materials, can realize simplifying with being prepared as local reduction and synthesis step.
It is an object of the invention to i.e. come from the rich of industry intermediate material containing the unpurified of the alloys such as Fe, S with itself
Rich and cheap positive metatitanic acid is as raw material, by the ratio of regulation and control hydrogen peroxide with positive metatitanic acid, organic acid and the ratio of positive metatitanic acid,
System titanium concentration, weak ammonia regulates the process conditions such as endpoint pH, prepares doping and can be easy to preservation steadily in the long term
Peroxo titanic acid sol, as intermediate, provides more convenient and possible for fields such as material preparation and photocatalysis.
Summary of the invention
The invention provides the positive metatitanic acid that a kind of employing prepared by industrial titanium sulphate solution is raw material, prepares stably-doped peroxide
The method of metatitanic acid colloidal sol: by the ratio of the ratio of regulation and control organic acid ('alpha '-hydroxy acids) with positive metatitanic acid, hydrogen peroxide and positive metatitanic acid,
System titanium concentration, regulation endpoint pH etc. prepares doping peroxo titanic acid sol.
The technical solution adopted for the present invention to solve the technical problems is implemented as follows:
(1) the titanic Acid precipitation containing the alloy such as ferrum, sulfur adding deionized water stirring and form suspension, amount of water is pressed
Following weight proportioning meter: titanic Acid precipitation 5-20 part, water 50-100 part；
(2) take 'alpha '-hydroxy acids and add suspension reaction；Wherein, during the addition of 'alpha '-hydroxy acids presses 'alpha '-hydroxy acids and positive metatitanic acid
The molar ratio computing of titanium: 'alpha '-hydroxy acids is at least 0.5 (preferably 'alpha '-hydroxy acids is 0.5-2 with the mol ratio of titanium) with the mol ratio of titanium；
(3) the turbid liquid after being complexed by alloy adds hydrogen peroxide, and hydrogen peroxide is more than 4 with the mol ratio of titanium, stirring
To clarification；Obtain the peroxo titanic acid sol that adulterates.
In preparation method of the present invention, the impact on preparation method of the present invention of the titanium concentration in the suspension of step (1) gained
It is: titanium concentration is the lowest more easily clarifies that concentration is the highest more the situation do not clarified easily occurs, but preparation method of the present invention is logical
Cross and proportionally add the organic acid such as 'alpha '-hydroxy acids and hydrogen peroxide controls its clarification degree.Alloy in titanic Acid precipitation, i.e.
Ferrum (soluble ferric iron salt) and sulfur (water dissolvable sulfur-containing compound), but it is not limited to ferrum (soluble ferric iron salt) and sulfur (water dissolvable
Sulfur-containing compound), also comprise other water dissolvable ion using the same manner to mix.
In the present invention, 'alpha '-hydroxy acids is to add suspension as stabilizer, present in the acid group of 'alpha '-hydroxy acids and system
Alloy ferrum and main body titanium ion generation complex reaction, form complex to eliminate dopant ions to peroxidating in subsequent process
The decomposition of hydrogen and the destruction of established pertitanic acid.Described 'alpha '-hydroxy acids typically uses citric acid, tartaric acid；Preferably employ lemon
Lemon acid.
In technique scheme, after step (3) stirring certain time, system is not yet clarified, then regulation pH value is to being clarified
System, obtain doping peroxo titanic acid sol.
Concrete, the scope of regulation pH value to 2-9, with clarification as Con trolling index.
Wherein, regulation pH value can use volatile ammonium salt, can be antacid, easily decomposes the alkaline matter of volatilization, it is to avoid
Introduce the material of the foreign ion that difficulty removes.Conventional such as ammonia, ammonium class carbonate or ammonium class sulphite etc..
By add above-mentioned substance (such as ammonia etc.) adjust pH value, alpha-hydroxy acid can be made to become anionic form, be conducive to and
Dopant ion and titanium ion complexation.
Wherein, the concentration of ammonia is generally 2%～25%.
Inventor forms fundamental reaction and the test portion screening employing peroxidating of complex according to titanium and hydrogen peroxide
Hydrogen reacts.Hydrogen peroxide (i.e. hydrogen peroxide) can be higher with titanium (IV) ion in solution or some reactivities titanium
Oxide, such as anatase titanium dioxide, metatitanic acid, (the strict reaction rate and anti-of controlling under suitable condition such as positive metatitanic acid
Answer heat release) carry out ligand complex reaction, make titanium dissolve dispersion with the form of the titanium hydrogen peroxide complex thing of Various Complex structure
Sol solutions is formed in water or other solvent.With this colloidal sol molten for predecessor can prepare easily follow-up variform containing titanizing
Laminate material.
It is an advantage of the current invention that: only need the addition of organic acid ('alpha '-hydroxy acids), the addition of hydrogen peroxide, mistake
Hydrogen oxide and the addition sequence of organic acid, the addition of pH adjusting agent (ammonia), be not required to just can obtain through complicated preparation technology
Must have the stable peroxo titanic acid sol of doping active component.Colloidal sol doping can realize the uniform mixing on molecular level, surely
Qualitative height, activity is high, and doping is flexibly.It is easy that the method has method, low cost, its lytic activity advantages of higher.According to the present invention
The method provided a step can prepare the doping poriferous titanium dioxide of anatase titanium dioxide crystal formation, bigger serface.
Present invention is expanded on further below in conjunction with embodiment, but these embodiments are not limiting as the protection model of the present invention
Enclose.
Detailed description of the invention
Below by reference to embodiment, the present invention is described in detail.It should be noted that used in the present invention
The positive metatitanic acid that adulterates be the alloy prepared by industrial titanium sulphate solution be ferrum (soluble ferric iron salt) and sulfur (water dissolvable sulfur-containing compound), but
It is not limited to ferrum (soluble ferric iron salt) and the positive metatitanic acid of doping of sulfur (water dissolvable sulfur-containing compound).
Embodiment 1
Take 10g to adulterate in positive metatitanic acid addition beaker, add 50 grams of deionized waters and stir, add 2.1g citric acid conduct
Stabilizer, reacts 1-3min, and pH value is 1.7.Being slowly added dropwise 10ml hydrogen peroxide as chelating agent, pH value is 2.0, stirs 3-5
Minute to clarification, pH value is 2.2, i.e. can get peroxo titanic acid sol.Gained peroxo titanic acid sol is placed and within more than 20 days, still may be used
Clear is stable.
Embodiment 2
Take 15g to adulterate in positive metatitanic acid addition beaker, add 50 grams of deionized waters and stir, add 3.15g citric acid and make
For stabilizer, reacting 1-3min, pH value is 1.6.Being slowly added dropwise 15ml hydrogen peroxide as chelating agent, pH value is 1.9, stirs 3-
Within 5 minutes, to clarification, pH value is 2.2, i.e. can get peroxo titanic acid sol.Gained peroxo titanic acid sol is placed and within more than 20 days, still may be used
Clear is stable.
Embodiment 3
Take 20g to adulterate in positive metatitanic acid addition beaker, add 100ml deionized water and stir, add 4.2g citric acid and make
For stabilizer, reacting 1-3min, pH value is 1.5.Being slowly added dropwise 20ml hydrogen peroxide as chelating agent, pH value is 1.8, stirs 3-
Within 5 minutes, to clarification, pH value is 2.2, i.e. can get peroxo titanic acid sol.Gained peroxo titanic acid sol is placed and within more than 20 days, still may be used
Clear is stable.
Embodiment 4
Take 10.03g to adulterate in positive metatitanic acid addition beaker, add 50 grams of deionized waters and stir, add 2.106g Fructus Citri Limoniae
Acid, as stabilizer, reacts 1-3min, and pH value is 1.8.Being slowly added dropwise 10ml hydrogen peroxide as chelating agent, pH value is 2.2, stirs
Mix 3-5 minute and do not clarify.After adding 5.2% ammonia 2.5ml, solution becomes clarification, and pH value is 5.56, i.e. can get pertitanic acid
Colloidal sol.Gained peroxo titanic acid sol is placed more than 20 days and still can stablize by clear.
Embodiment 5
Take 14.98g to adulterate in positive metatitanic acid addition beaker, add 50 grams of deionized waters and stir, add 3.35g citric acid
As stabilizer, reacting 1-3min, pH value is 1.7.Being slowly added dropwise 17ml hydrogen peroxide as chelating agent, pH value is 2.1, stirring
Within 3-5 minute, not clarifying, after adding 25% ammonia 0.8ml, solution becomes clarification, and pH value is 5.9, i.e. can get pertitanic acid molten
Glue.Gained peroxo titanic acid sol is placed more than 20 days and still can stablize by clear.
Embodiment 6
Peroxo titanic acid sol liquid (after Room-temperature seal stands 30 days) in Example 2, uses dip-coating method in cleaning
Masking on common glass sheet.Membrane speed 5cm/min, infrared lamp is dried 5min and is placed in drying baker 100 DEG C and continues to be dried
Repeat after 30min to lift five times.In Muffle furnace, 5 DEG C/min is warming up to 450 DEG C of insulation 30min preparation doping the most after drying
Titanium deoxid film.It has at room temperature reached 98% with after degradation rate 90min to 5mg/L methyl orange under ultra violet lamp.
With reference to said method, Example 1, titania-doped thin film prepared by 3-5 gained peroxo titanic acid sol liquid is also
Meet related degradation standard.
Embodiment 7
Peroxo titanic acid sol liquid (after room temperature stands 25 days) in Example 5, transfers to constant-temperature vacuum and does after stirring
Dry case is evaporated to dryness gel in 50 DEG C.It is warming up to 450 DEG C of insulation 30min with 5 DEG C/min after mortar is finely ground, obtains Doped Nanosize
Miscellaneous titanium dioxide powder, its particle diameter 30-50nm.
With reference to said method, mixed nanometer titanium dioxide powder prepared by Example 1-4 gained peroxo titanic acid sol liquid is also
Meet relevant particle diameter demand.
To sum up, the invention provides a kind of method that cheap raw material prepares stably-doped peroxo titanic acid sol, made
Prepare doping poriferous titanium dioxide for intermediate or utilize pertitanic acid to modify, solving to prepare at present the porous dioxy that adulterates
The cost of material changing titanium is high, complicated process of preparation, the problems such as performance is low.It is characterized in being existed by the mass fraction of the positive metatitanic acid of regulation and control
Certain limit, system titanium concentration, the addition of hydrogen peroxide, the addition of organic acid, hydrogen peroxide are suitable with the addition of organic acid
Sequence, the parameter such as addition of ammonia regulate endpoint pH, it is thus achieved that have the stable peroxo titanic acid sol of doping active component.
The doping pertitanic acid using the method to prepare is orange red and yellow transparent colloidal dispersion, and colloidal sol doping can realize molecular level
On mixing, stability is high, and activity is high, and doping is flexibly；It is easy that the present invention has method, low cost, its lytic activity advantages of higher.
Use peroxo titanic acid sol of the present invention a step can prepare the doping poriferous titanium dioxide of anatase crystal, bigger serface.
Claims (10)
- The preparation method of the most stably-doped peroxo titanic acid sol, it is characterised in that: comprise the following steps:(1) the titanic Acid precipitation containing alloy adding deionized water stirring and form suspension, amount of water is joined by following weight Than meter: titanic Acid precipitation 5-20 part, water 50-100 part；(2) take 'alpha '-hydroxy acids and add suspension reaction；Wherein, the addition of 'alpha '-hydroxy acids presses 'alpha '-hydroxy acids and titanium in positive metatitanic acid Molar ratio computing: 'alpha '-hydroxy acids is at least 0.5 with the mol ratio of titanium；(3) the turbid liquid after being complexed by alloy adds hydrogen peroxide, and hydrogen peroxide is more than 4 with the mol ratio of titanium, and stirring is to the most clear Clearly；Obtain the peroxo titanic acid sol that adulterates.
- The preparation method of stably-doped peroxo titanic acid sol the most according to claim 1, it is characterised in that: step (2) The addition of described 'alpha '-hydroxy acids is by the molar ratio computing of titanium in 'alpha '-hydroxy acids and positive metatitanic acid: 'alpha '-hydroxy acids with the mol ratio of titanium is 0.5-2。
- The preparation method of stably-doped peroxo titanic acid sol the most according to claim 1 and 2, it is characterised in that: described 'alpha '-hydroxy acids is citric acid, tartaric acid.
- The preparation method of stably-doped peroxo titanic acid sol the most according to claim 3, it is characterised in that: described α-hydroxyl Base acid is for preferably employing citric acid.
- The preparation method of stably-doped peroxo titanic acid sol the most according to claim 1, it is characterised in that: step (3) If stirring certain time after system not yet clarify, then regulation pH value to obtain clarification system, obtain doping peroxo titanic acid sol.
- The preparation method of stably-doped peroxo titanic acid sol the most according to claim 5, it is characterised in that: regulation pH value In the range of 2-9, with clarification for controlling terminal.
- The preparation method of stably-doped peroxo titanic acid sol the most according to claim 5, it is characterised in that: regulation pH value Use volatile ammonium salt, can be antacid, easily decompose the alkaline matter of volatilization, it is to avoid introduce the thing of the foreign ion that difficulty removes Matter.
- The preparation method of stably-doped peroxo titanic acid sol the most according to claim 5, it is characterised in that: regulation pH value Use ammonia, ammonium class carbonate or ammonium class sulphite.
- The preparation method of stably-doped peroxo titanic acid sol the most according to claim 8, it is characterised in that: regulation pH value Use ammonia.
- 10. the preparation method described in any one of claim 1-9 prepares the stably-doped peroxo titanic acid sol of gained.
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Cited By (4)
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| CN110250169A (en) * | 2019-05-06 | 2019-09-20 | 厦门威亮光学涂层技术有限公司 | A kind of Ag-carried nanometer titanium dioxide colloidal sol and its preparation method and application |
| CN111170282A (en) * | 2020-01-07 | 2020-05-19 | 北京科技大学 | Preparation method of inorganic peroxotitanic acid dispersant |
| CN111792670A (en) * | 2020-06-22 | 2020-10-20 | 佛山欧神诺陶瓷有限公司 | Titanium dioxide photocatalyst, preparation method thereof and application thereof in ceramic tiles |
| CN114097821A (en) * | 2021-11-17 | 2022-03-01 | 杭州大岸科技有限公司 | Sterilization disinfectant and preparation method and application thereof |
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| CN110250169A (en) * | 2019-05-06 | 2019-09-20 | 厦门威亮光学涂层技术有限公司 | A kind of Ag-carried nanometer titanium dioxide colloidal sol and its preparation method and application |
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| CN114097821A (en) * | 2021-11-17 | 2022-03-01 | 杭州大岸科技有限公司 | Sterilization disinfectant and preparation method and application thereof |
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