CN102086047B - Titanium dioxide powder with ultrahigh water dispersion and high photocatalytic activity and preparation method thereof - Google Patents
Titanium dioxide powder with ultrahigh water dispersion and high photocatalytic activity and preparation method thereof Download PDFInfo
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- CN102086047B CN102086047B CN2011100049122A CN201110004912A CN102086047B CN 102086047 B CN102086047 B CN 102086047B CN 2011100049122 A CN2011100049122 A CN 2011100049122A CN 201110004912 A CN201110004912 A CN 201110004912A CN 102086047 B CN102086047 B CN 102086047B
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Abstract
The invention relates to titanium dioxide powder with ultrahigh water dispersion and high photocatalytic activity and a preparation method thereof. The method comprises the following steps: adding titanium salt in alcohol solvent to prepare precursor, performing low-temperature non-aqueous solvent heat treatment to the precursor, washing the product with ethanol, centrifuging, and drying to obtain titanium dioxide powder with ultrahigh water dispersion and high photocatalytic activity. The obtained titanium dioxide belongs to anatase polycrystal and consists of 5-10nm of particles; the isoelectric point of titanium dioxide is 6.3; when the pH value is less than 5 or more than 6.5, the absolute value of the Zeta potential is more than 30 millivolts; the weight percentage of titanium dioxide is 0.1%-50%, the aqueous dispersion can remain stable for at least 48 hours; and the pollutants can be completely degraded in 1 hour under the simulated sunlight. The method of the invention has simple synthetic route, controllable technological process, low reaction temperature, accessible raw materials, low cost and high yield which is up to 97% and is suitable for industrial mass production.
Description
Technical field
The present invention relates to a kind of anatase titania powder that has superelevation dispersiveness and highlight catalytic active simultaneously and preparation method thereof; Adopt the preparation of non-aqueous sol-gel method; Resulting anatase titania powder not only has very high photocatalytic activity, and can be with 50% mass concentration stable dispersion in water.
Background technology
The titanium dioxide stable in properties, nontoxic, production cost is low, is a kind of broad-spectrum commerical prod, as pigment, coating, the additive of ointment etc.From 1972; Two professors of the Fujishima of Tokyo Univ Japan and Honda find that rutile titanium dioxide monocrystalline electrode produces electromotive force under the xenon lamp irradiation; Brine electrolysis generates hydrogen, shows that titanium oxide can change luminous energy into be stored in the hydrogen chemical energy [Fujishima A, Honda K.Electrochemical photocatalysisof water at a semiconductor electrode Nature 1972; 238,37].This discovery has started the upsurge of conductor photocatalysis research at once, and titanium oxide has received people's extensive concern as a kind of novel photocatalyst material.Development along with and nanometer science and technology deep gradually to the research of titanium oxide; Nano titanium oxide shows increasing advantage; Nano titanium oxide can be used as effective novel photocatalysis agent, anti UV agent, photovoltaic effect agent etc., shows wide application prospect in fields such as antibacterial and mouldproof, exhaust gas purification, deodorization, water treatment, antifouling, weather-proof anti-aging, automobile finishs.
Research to titanium oxide at present mainly concentrates on the powder; The research of relevant its aqueous dispersions is less, and dispersing nanometer titanium dioxide liquid has purposes more widely, and nano titanium oxide is scattered in the water; Particle more approaches initial size; Solved some difficult problems that exist when using powder, as be difficult for being uniformly dispersed, end-use performance is not high.At present; Fewer to the research report of nano-titanium dioxide powder ability stable dispersion in water, people's spent glycols such as Guo are made solvent, the hydrolysis of control titanium tetrachloride; Synthesized the nanometer sheet with square and hexagonal titanium oxide, this titanium oxide can be dispersed in the water well.Find that after deliberation in reaction process, the formation of titanium dioxide nanoplate is relevant with the auxiliary precipitation-peptization of the rate of release of water and hydrochloric acid.Terepthaloyl moietie pyrolysated product; Like aldehydes etc., be combined on the titanium oxide, can prevent the reunion of titanium dioxide nanoplate; Therefore make it can well be dispersed in [Guo B.S., Demopoulos G.P.Thesynthesis of aqueous-dispersible anatase TiO in the water
2Nanoplatelets Nanotechnology 2010,21,1-9].
Adopt same principle, people such as Wang are with metatitanic acid four Virahol esters, and terepthaloyl moietie and nano level pure water are raw material, and 150 ℃ were reacted 2 hours, can obtain the titanium dioxide nano-particle that particle diameter is about 2nm, and this titanium oxide has good photoelectric property.Because institute's synthetic titanium dioxide surface has been modified glycol molecule, this nanoparticle can well be dispersed in water and the ethanol, can stablize to keep at least 10 days.But employed method relative complex such as Du; Add water amount need strict control; As adding water, just can not synthesize anatase titania [Wang P., Wang D.J. with polymolecularity not according to ratio described in the literary composition; Li H.Y, et al.A facile solution-phase synthesis of high quality water-soluble anatase TiO
2Nanocrystals J.ColloidInterface Sci.2007,314,337-340].
Except above method, also there is the investigator to be utilized in titanium dioxide surface and modifies organic molecule, make titanium dioxide nano-particle ability stable dispersion in certain solvent.Such as, Imae etc. have studied titanium oxide the dispersiveness in water relevant with the pH value of solution value, under the existence condition of tensio-active agent, under situation about existing in sodium lauryl sulphate, can improve the dispersiveness of titanium oxide under neutrallty condition; And in the presence of dimethyl dodecyl amine oxide, can improve the dispersiveness of titanium oxide under acidity or alkaline condition.The investigator has also studied the reason of the dependency of dispersability of titanium dioxide and pH, and its reason mainly is the tensio-active agent that is adsorbed on titanium dioxide surface, or forms hemimicelle; Or the two electric compressive layers of formation; Make its can be in the solution of different pH values stable dispersion [Imae T., Muto K., Ikeda S.The pH dependence ofdispersion of particles in aqueous surfactant solutions Colloid.Polym.Sci.1991; 269,43-48].
People such as Niederberger adopt method enediol equimolecular in the titanium dioxide nano-particle finishing of in-situ modification; Like Dopamine HCL; P-ten.-butylcatechol makes that institute synthetic nano titanium oxide can stable dispersion [Niederberger M., Garnweitner G. in water and organic solvent; Krumeich F.; Et al.Tailoring the surface and solubillityproperties of nanocrystalline titania by a nonaqueous in situ functionalization process Chem.Mater.2004,16,1202-1208].
More than in several pieces of documents the titanium oxide of reporting high-dispersed all are the corresponding organic molecules that derived from its surface adsorption; And in the present invention, the applicant adopts a kind of low temperature non-aqueous sol-gel method that need not to add any tensio-active agent to synthesize to possess highly active water-soluble titanium oxide.The titanium dioxide surface of gained does not have organic molecule to be modified, but can mix by a certain percentage with water, obtains the stabilize water dispersion liquid of different concns.Simultaneously, by the titania powder good crystallinity that this reaction obtains, size distribution is even, has good photocatalytic activity, under the simulated solar rayed, can realize the degraded fully to target contaminant (rhodamine B) in about 1 hour.Whole production technology is simple, operation easily, and synthesis temperature is low; Do not have complicated subsequent disposal, reaction yield is up to 97%, and industry amplification influence factor is little; Cost is low, is the superelevation water dispersible, and the suitability for industrialized production of high reactivity property titanium dioxide powder photocatalyst provides a feasible approach.
Summary of the invention
The object of the invention aims to provide a kind of titanium dioxide powder with superelevation water dispersible and highlight catalytic active and preparation method thereof.
For realizing above-mentioned purpose, technical scheme of the present invention is:
A kind of titanium dioxide powder with superelevation water dispersible and highlight catalytic active; It is characterized in that this powder is the anatase titania polycrystalline, by the granulometric composition of size at 5～10nm; The iso-electric point of its titanium oxide is 6.3; Less than 5 or greater than 6.5 o'clock, the absolute value of Zeta potential is all greater than 30 millivolts in the pH value, and the titanium oxide mass percent concentration is that 0.1%～50% aqueous dispersions can be stablized maintenance at least 48 hours; Under the simulated solar rayed, can realize degraded fully in 1 hour to pollutent.
Preparing method with titanium dioxide powder of superelevation water dispersible and highlight catalytic active of the present invention is characterized in that, adopts the preparation of low temperature non-aqueous sol-gel method, and preparation process is followed successively by:
Step 1: in alcoholic solvent, add titanium salt, be configured to presoma, the amount of titanium salt is 0.1～1.5 mol;
Step 2: the presoma that is configured to that obtains in the step 1 is carried out solvent heat treatment, 100～250 ℃ of treatment temps, the time is 6～48 hours;
Step 3: centrifugal after the reaction of step 2 finishes, and with the centrifugal product that obtains with washing with alcohol more than 3 times, product promptly obtains possessing the titanium dioxide powder of superelevation water dispersible highlight catalytic active 20-150 ℃ of air drying 12 hours.
Wherein, described titanium salt is titanium tetrachloride, metatitanic acid four Virahol ester or tetrabutyl titanates;
Described alcohols is methyl alcohol, ethanol, Virahol, propyl carbinol, isopropylcarbinol, terepthaloyl moietie, Ucar 35, glycerine or phenylcarbinol.
Described titanium salt is titanium tetrachloride, metatitanic acid four Virahol ester or tetrabutyl titanates; Above-mentioned alcohols is methyl alcohol, ethanol, Virahol, propyl carbinol, terepthaloyl moietie, Ucar 35, glycerine or phenylcarbinol.
The invention has the advantages that:
1, the synthetic titanium deoxide catalyst can very stable being dispersed in the water.
2, this titanium dioxide optical catalyst has good photocatalytic activity, under the simulated solar rayed, can realize in 1 hour to pollutent near 100% degraded.
3, entire synthesis process is carried out at low temperatures, and technological process is simple, and industrial amplification factor is little, and productive rate is high, without any need for the thermal treatment subsequent step, meets very much demand of practical production.
Description of drawings
Fig. 1 is the XRD figure spectrum of prepared titanium oxide
The picture in picture spectrum is corresponding to anatase titania (JCPDS No.71-1167).
Fig. 2 is prepared corresponding TEM (figure A) and the HRTEM figure (B figure) of titanium oxide
Illustration is the SEAD figure of this sample among the figure A figure.
Can draw following information from TEM figure, the prepared titanium oxide of the present invention is polycrystalline, and by the granulometric composition of size at 5～10nm, size distribution is more even.Can find out that from HRTEM this titanium oxide crystallinity is fine.
Fig. 3 is the prepared Zeta potential of titanium oxide dispersion (mass percent concentration is 0.1%) under different pH values
As can be seen from the figure, the iso-electric point of prepared titanium oxide is about 6.3, and less than 5 or greater than 6.5 o'clock, the absolute value of Zeta potential shows that all greater than 30 millivolts the equal ability of titanium oxide stable dispersion is in water in the pH value.
Fig. 4 is the photo in kind of the titanium dioxide water-dispersion liquid of different concns
The dispersion liquid of the titanium oxide that the present invention is prepared, mass percent concentration is respectively 0.1%, 1%, and 5%, 10%, 30%, 50% can stablize maintenance at least 48 hours.Obvious sedimentation promptly takes place after leaving standstill 1 hour and mass percent concentration is the aqueous dispersions of 0.1% Degussa P25.
Fig. 5 is the fourier transform infrared spectrometry figure of prepared titanium oxide
Can find out that by this figure prepared titanium dioxide surface does not have organic group.
Fig. 6 is under the simulated solar rayed, and prepared titanium oxide and commercially available Degussa P25 are to the degradation curve of rhodamine B
As can be seen from the figure, prepared titanium oxide (is used TiO among the figure
2Mark) has good photocatalytic activity, under the simulated solar rayed, can realize degraded fully in about 1 hour pollutent.And under equal conditions, commercially available Degussa P25 only can degrade about 30%.
Embodiment
Have the titanium dioxide powder preparation of superelevation water dispersible and highlight catalytic active, preparation process is:
Step 1: in phenylcarbinol, add titanium tetrachloride, be configured to presoma, the amount of titanium tetrachloride is 0.5 mol;
Step 2: the presoma of step 1 is carried out solvent heat treatment, and treatment temp is 180 ℃, and the time is 20 hours;
Step 3: centrifugal after step 2 finishes, and with the centrifugal product that obtains with washing with alcohol 3 times, product promptly obtains possessing the titanium dioxide powder of superelevation water dispersible highlight catalytic active 50 ℃ of air dryings 12 hours.
Have the titanium dioxide powder preparation of superelevation water dispersible and highlight catalytic active, preparation process is:
Step 1: in phenylcarbinol, add metatitanic acid four Virahol esters, be configured to presoma, the amount of isopropyl titanate is 0.3 mol;
Step 2: the precursor liquid of step 1 is carried out solvent heat treatment, and treatment temp is 200 ℃, and the time is 20 hours;
Step 3: centrifugal after step 2 finishes, and with the centrifugal product that obtains with washing with alcohol 3 times, product promptly obtains possessing the titanium dioxide powder of superelevation water dispersible highlight catalytic active 120 ℃ of air dryings 12 hours.
Embodiment 3
Have the titanium dioxide powder preparation of superelevation water dispersible and highlight catalytic active, preparation process is:
Step 1: in phenylcarbinol, add tetrabutyl titanate, the amount that is configured to the presoma tetrabutyl titanate is 0.1 mol
Step 2: the presoma of step 1 is carried out solvent heat treatment, and treatment temp is 250 ℃, and the time is 20 hours;
Step 3: centrifugal after step 2 finishes, and with the centrifugal product that obtains with washing with alcohol 3 times, product promptly obtains possessing the titanium dioxide powder of superelevation water dispersible highlight catalytic active 50 ℃ of air dryings 12 hours.
Embodiment 4
Have the titanium dioxide powder preparation of superelevation water dispersible and highlight catalytic active, preparation process is:
Step 1: in ethanol, add titanium tetrachloride and be configured to presoma, the amount of titanium tetrachloride is 0.9 mol;
Step 2: the presoma of step 1 is carried out solvent heat treatment, and treatment temp is 120 ℃, and the time is 24 hours;
Step 3: centrifugal after step 2 finishes, and with the centrifugal product that obtains with washing with alcohol 3 times, product promptly obtains possessing the titanium dioxide powder of superelevation water dispersible highlight catalytic active 150 ℃ of air dryings 12 hours.
Have the titanium dioxide powder preparation of superelevation water dispersible and highlight catalytic active, preparation process is:
Step 1: in terepthaloyl moietie, add titanium tetrachloride and be configured to presoma, the amount of titanium tetrachloride is 1.0 mol;
Step 2: the presoma of step 1 is carried out solvent heat treatment, and treatment temp is 180 ℃, and the time is 18 hours;
Step 3: centrifugal after step 2 finishes, and with the centrifugal product that obtains with washing with alcohol 3 times, product promptly obtains possessing the titanium dioxide powder of superelevation water dispersible highlight catalytic active 50 ℃ of air dryings 12 hours.
Have the titanium dioxide powder preparation of superelevation water dispersible and highlight catalytic active, preparation process is:
Step 1: in methyl alcohol, add titanium tetrachloride, the amount that is configured to the presoma titanium tetrachloride is 1.2 mol;
Step 2: the presoma of step 1 is carried out solvent heat treatment, and treatment temp is 100 ℃, and the time is 24 hours;
Step 3: centrifugal after step 2 finishes, and with the centrifugal product that obtains with washing with alcohol 3 times, product promptly obtains possessing the titanium dioxide powder of superelevation water dispersible highlight catalytic active 100 ℃ of air dryings 12 hours.
Embodiment 7
Have the titanium dioxide powder preparation of superelevation water dispersible and highlight catalytic active, preparation process is:
Step 1: in Virahol, add titanium tetrachloride, be configured to presoma, the amount of titanium tetrachloride is 0.8 mol;
Step 2: the presoma of step 1 is carried out solvent heat treatment, and treatment temp is 220 ℃, and the time is 24 hours;
Step 3: centrifugal after step 2 finishes, and with the centrifugal product that obtains with washing with alcohol 3 times, product promptly obtains possessing the titanium dioxide powder of superelevation water dispersible highlight catalytic active 50 ℃ of air dryings 12 hours.
Have the titanium dioxide powder preparation of superelevation water dispersible and highlight catalytic active, preparation process is:
Step 1: in propyl carbinol, add titanium tetrachloride, be configured to presoma, the amount of titanium tetrachloride is 0.5 mol;
Step 2: the presoma of step 1 is carried out solvent heat treatment, and treatment temp is 190 ℃, and the time is 36 hours;
Step 3: centrifugal after step 2 finishes, and with the centrifugal product that obtains with washing with alcohol 3 times, product promptly obtains possessing the titanium dioxide powder of superelevation water dispersible highlight catalytic active 50 ℃ of air dryings 12 hours.
Claims (1)
1. have the preparation method of the titanium dioxide powder of superelevation water dispersible and highlight catalytic active, it is characterized in that, adopt the preparation of low temperature non-aqueous sol-gel method, preparation process is followed successively by:
Step 1: in ethanol, add titanium tetrachloride, be formulated as presoma, the amount of titanium tetrachloride is 0.1～1.5 mol;
Step 2: the presoma that obtains in the step 1 is carried out solvent heat treatment, 100～250 ℃ of treatment temps, the time is 6～48 hours;
Step 3: after the reaction of step 2 finishes; Centrifugal, and with the centrifugal product that obtains with washing with alcohol more than 3 times, product was 20～150 ℃ of air dryings 12 hours; Promptly obtain possessing the titanium dioxide powder of superelevation water dispersible highlight catalytic active; This powder is the anatase titania nano particle, and size is in 5～10 nanometers, and the titanium oxide mass percent concentration is that 0.1%～50% aqueous dispersions can be stablized maintenance at least 48 hours.
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| CN116212843B (en) * | 2023-02-14 | 2024-01-19 | 甘肃自然能源研究所 | Preparation method and application of self-template capable of realizing structural regulation and control of flower-like, hollow and solid titanium dioxide microspheres |
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