CN105523583A - Synthetic method of nano titanium dioxide powder - Google Patents
Synthetic method of nano titanium dioxide powder Download PDFInfo
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- CN105523583A CN105523583A CN201410563857.4A CN201410563857A CN105523583A CN 105523583 A CN105523583 A CN 105523583A CN 201410563857 A CN201410563857 A CN 201410563857A CN 105523583 A CN105523583 A CN 105523583A
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Abstract
The invention discloses a synthetic method of nano anatase titanium dioxide powder. The method comprises the following steps: 1) dropping a titanium oxide precursor in water, performing a hydrolysis reaction to obtain white precipitate, after reaction is completed, obtaining a solid-liquid mixture; 2) adding an alkyl ammonium hydroxide solution in the mixture obtained in the step 2), uniformly mixing the materials and aging the materials; and 3) adding a glacial acetic acid solution in the aged product obtained in the step 2), performing a constant temperature reaction, after the reaction is completed, separating the product, cleaning the product and drying the product to obtain the nanometer titanium dioxide powder. The method has the advantages of simple process, low synthesis temperature, mild condition, easy operation and high output, the size of the prepared titanium oxide nanoparticle is small, and the method is suitable for preparing a catalyst for selective catalytic denitration or a photocatalysis.
Description
Technical field
The invention belongs to nano material synthesis field, relate to a kind of synthetic method of anatase octahedrite nanometer titanium dioxide titanium valve particularly.
Background technology
Usually, the preparation method of titanium dioxide powder has two kinds, and one is sulfuric acid process, chlorination process, and the method for traditional titanium dioxide synthesis is sulfuric acid process, but sulfuric acid process environmental pollution is serious, and equipment loss is serious, and the method that is chlorinated gradually replaces.Sulfuric acid process can be produced and comprise anatase structured and titanium dioxide powder that is rutile structure; And chlorination process can only produce the titanium dioxide powder of rutile.Current anatase structured titanium dioxide powder, except having except important application in photochemical catalysis, also occupies the very large SCR market share, and application prospect is very good, therefore, develops low cost, and high performance titanium dioxide powder preparation technique has very high using value.
TiO
2synthetic method is very many, substantially can be divided into vapor phase process and liquid phase method.Vapor phase process is by TiCl
4steam and oxygen react instantaneously at high temperature, obtained titanium dioxide powder, and this methods experiment condition is harsh, needs temperature high, strong to equipment corrosion, is seldom used.It is actual that to adopt maximum be liquid phase method, early application be the precipitator method, sol-gel method, can be easy to obtain nanoscale ti powder, and industrial continuous seepage can be realized.As patent CN97108439.4 discloses a kind of homogeneous precipitation method, obtain titanium dioxide with metatitanic acid and urea coprecipitation, after roasting, form nano-titanium oxide.But the titanium oxide that these methods obtain is all atypic titanium oxide, through further pyroprocessing, crystalline phase titanium dioxide must be formed.And the titanium oxide formed is without fixing form, easily reunites.
Microemulsion method, hydrothermal synthesis method can control the pattern of titanium dioxide, as patent CN200810239755.1 discloses a kind of hydrothermal synthesis method of TiOx nano band, take titanium oxide powder as titanium source, 160 DEG C ~ 200 DEG C reaction for some time in the strong base solution such as NaOH or KOH of ethanol, the product of band shape just can be obtained.Shortcoming is that product size is too large, and strip length reaches micron order, and width also has tens nanometers.The nano level that the current titanium dioxide being photochemical catalysis or SCR catalyst need is all, the titanium dioxide that obvious this method obtains is not suitable for application in this regard.CN101468812 discloses a kind of synthetic method of titanium dioxide nano-rod, by titanium valve and dehydrated alcohol, and CCl
4strong base solution Deng organic solvent mixes, adopt microwave heating method can Fast back-projection algorithm TiOx nano rod, excellent length 150-200nm, diameter 10 nanometer.But microwave heated samples treatment capacity is low, and the Titanium particles size obtained is large too.
CN200910040400.4 discloses a kind of method of precipitator method synthesis of titanium dioxide colloid, with titanyl sulfate as presoma, regulate pH to alkalescence with ammoniacal liquor, use hydrogen peroxide adjust ph to acid again, the fusiformis titania nanoparticles of polymolecularity can be obtained, selected by be the pattern that the most easily occurs of synthesis titanium oxide, surface with step-like exposed, has lower activity with (101) face.
CN200810231723.7 discloses a kind of titanium dioxide hydrothermal synthesis method, adds the carboxylic acid aqueous solution containing mercapto groups, solution is placed in reactor in the ethanolic soln of positive four butyl esters of metatitanic acid, at the 210-300 DEG C of obtained nano titanium oxide of reaction.The method synthesis reaction temperature is high, with ethanol as solution, produces very large pressure, harsh to equipment requirements.Yanghuagui article (Nature, 2008,453:638) reports a kind of lamella micro-scale titanium dioxide crystal, and feature is main exposed with (001) face, and size is single, and brings the upsurge of titanium dioxide crystal morphology control.Its building-up process in HF solution, with the Hydrothermal Synthesis of titanium tetrafluoride as presoma.
CN200910110851.0 discloses one in a solution of hydrofluoric acid, with titanium isopropylate as titania precursor body, forms the synthetic method of nano-titanium oxide lamella.As can be seen from above, although Hydrothermal Synthesis can the pattern of controlled oxidization titanium, be all at strong acid or strong base solution as solvent, not easily reclaim, there is very strong corrodibility, cause environmental pollution.Except hydrothermal method; the solvent-thermal method taking organic solution as solvent can the pattern of controlled oxidization titanium; if WuBinghui is at document (J.Amer.Chem.Soc.2008; 130,12597) report in phenylcarbinol as solvent, temperature is at 160 DEG C; the uniform nanometer anatase titania of appearance can be obtained under protective material effect; crystal appearance is prismatic, is main exposed surface, has very high photodegradation with (100) face.But the cost of the cost of organic solvent and subsequent disposal is higher.
CN1935669A discloses a kind of low temperature synthesis of anatase octahedrite nano titanium oxide, after sulfuric acid dissolution ilmenite, titanic Acid precipitation is formed by basic solution precipitation, again positive metatitanic acid is disperseed with hydrogen peroxide, with acid for adjusting pH value, make the one-tenth of solution acid, titanium dioxide powder or titanium oxide sol can be obtained according to demand.Obtain the grain-size of titanium dioxide powder in 40 ~ 60 nanometers.
CN103121711A discloses a kind of synthetic method of full titania nanoparticles, after metatitanic acid organic salt is mixed with dehydrated alcohol, add water and make colloidal sol, bicarbonate of ammonia is added by colloidal sol, grain-size can be obtained single after hydrothermal treatment consists, crystal formation is anatase structured titanium dioxide powder, and size is in 8 ~ 12 nanometers.The titanium dioxide pattern of the method synthesis is irregular, and has part to reunite, and synthesis temperature is higher.
" artificial lens journal " the 6th phase in 2006, " hydrothermal method prepared Anatase TiO
2nanocrystalline " in a literary composition, with tetraethyl ammonium hydroxide (TENOH) for peptizing agent and butyl (tetra) titanate (TNB) are for presoma, take Virahol as solvent, adopt hydrothermal method to obtain a series of TiO at a higher temperature
2nanocrystalline.The method Virahol is as solvent, and hydrothermal temperature is more than 150 DEG C.Temperature is higher, and the titania size obtained is comparatively large, more than 100 nanometers.
As can be seen to above patent and document analysis, from unformed powder to size and morphology controllable synthesis of nano particle, be the general trend of titanium dioxide study on the synthesis.Common hydrothermal method can realize the morphology control of titanium dioxide, but the many employings of open material in the past have the acid of severe corrosive or alkali as solvent, and temperature of reaction is high, operates more dangerous, may work the mischief to equipment and experimenter.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of synthetic method of nano-titanium dioxide powder, the nanometer titanium dioxide titanium valve that the method is obtained, size uniform, pattern is single, has good water and ethanol dispersiveness, synthesis temperature is low, simple to operate, is suitable for industrial production.
The synthetic method of a kind of nano-titanium dioxide powder provided by the invention, comprises the following steps:
(1) be added drop-wise in water by the presoma of titanium oxide under agitation condition, be hydrolyzed reaction, generates white precipitate, and white precipitate, through being separated, cleaning, is re-dispersed in water, obtains solidliquid mixture;
(2) in the mixture of step (1), add alkyl phosphonium hydroxide ammonium solution, mix, aging;
(3) add glacial acetic acid solution, isothermal reaction in step (2) ageing products, after reaction terminates, reaction product, through being separated, cleaning and drying, obtains nanometer titanium dioxide titanium valve.
According to method of the present invention, wherein the titania precursor body described in step (1) is selected from one or more in titanium tetrachloride, titanium sulfate and Organic Alcohol oxygen titanium; Wherein Organic Alcohol oxygen titanium is one or more of titanium isopropylate, tetrabutyl titanate or titanium isopropylate.
The mol ratio of the water described in step (1) and titanium is 10 ~ 100, preferably 10 ~ 15.
Cleaning described in step (1) is that its process be by after product and distilled water by volume 1:3 ~ 1:6 mixing and stirring, carries out suction filtration separation or centrifugation with distilled water cleaning, preferred suction filtration separation, above process repetition 2 ~ 5 times.
Dispersion described in step (1) is by H
2o/Ti mol ratio is 80 ~ 120, disperses with stirring or ultrasonic power.
The whole process of step (1) is generally at room temperature carried out.
Alkyl ammonium hydroxide described in step (2) is selected from one or more in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH or TBAH, preferred Tetramethylammonium hydroxide.The concentration of alkyl phosphonium hydroxide aqueous ammonium is generally 10wt% ~ 40wt%.
The add-on of alkyl ammonium hydroxide described in step (2) is with the molar ratio computing of ammonium and titanium lower than 1, and preferred molar ratio is 0.3 ~ 0.7.
Aging temperature described in step (2) is 50 ~ 90 DEG C of interval arbitrary temperature, preferably 70 ~ 80 DEG C, is more preferably 80 DEG C; Described digestion time is 10 ~ 30 hours, is preferably 16 ~ 30 hours.
Adding glacial acetic acid amount described in step (3), is 0.5 ~ 2 by acetic acid/Ti mol ratio; Isothermal reaction is generally carried out in autoclave, can be static reaction still or dynamic response still.
Temperature of reaction described in step (3) is 120 ~ 220 DEG C of interval arbitrary temperature, is preferably 120 ~ 140 DEG C; The described reaction times is 10 ~ 30 hours, is preferably 20 ~ 24 hours.
Separation described in step (3), cleaning and drying can adopt the routine operation in this area.Can adopt centrifugation as separation method, centrifugation rotating speed is generally 4000 ~ 7000rpm.The condition of step (3) described cleaning is generally: isolated solid is adopted ultrasonic disperse in deionized water, and adopt centrifugation to be separated, centrifugation rotating speed is generally 7000 ~ 12000rpm.Described drying conditions is generally: in air atmosphere at 50 ~ 120 DEG C of temperature dry 10 ~ 30 hours.
The nanometer titanium dioxide titanium valve prepared according to the inventive method, having following characteristics is: titanium dioxide has anatase structured, and size range is 10-20nm, and specific surface area is 100 ~ 150m
2/ g, formed and pile up meso-hole structure, mesopore size is at 8-10nm.Titanium dioxide has good water and ethanolic soln is dispersed.
The present invention adopts organic bases as the protective material reacted and pH value regulator; titanium salt hydrolysis forms titanium hydroxide precipitation; peptization is there is in the organic bases treating processes of comparatively high temps; add glacial acetic acid in the solution afterwards; the effect of glacial acetic acid be not titanium salt hydrolysis inhibitor but as surperficial selective agent; be adsorbed on some feature crystal faces of titanium dioxide, hinder crystal face growth, form the titania nanoparticles of tetrahedron profile.The inventive method is simple, and synthesis temperature is low, and reaction conditions is loose, easy handling, and output is large, and productive rate is high, is suitable for industrial production.The product obtained is Nano titanium dioxide powder, is suitable as the support of the catalyst of selective catalytic reduction flue gas denitration reaction.
Compared with prior art, the synthetic method of titanium dioxide powder provided by the invention, has following characteristics:
1, the nanometer titanium dioxide titanium valve that the inventive method is obtained, size uniform, pattern is single, has good water and ethanol dispersiveness.
2, the synthesis of titanium dioxide powder method of the present invention's employing, reaction conditions is loose, simple to operate, and output is large, is suitable for industrial production.
3, the TiO synthesized with prior art
2nanocrystallinely compare, the nanometer titanium dioxide titanium valve synthesized by the inventive method, the temperature of synthesis is low, and crystallization is good, and crystal grain is in 10-20nm scope, and specific surface area reaches 100 ~ 150m
2/ g, such titanium dioxide powder is applicable to the catalyzer doing light-catalyzed reaction and the selective catalytic denitrification process reaction.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction spectrogram of the titanium dioxide according to embodiment 1 preparation.
Fig. 2 is the transmission electron microscope photo of the titanium dioxide according to embodiment 1 preparation.
Embodiment
The preparation process of titanium dioxide nanocrystalline in the present invention is further illustrated below with specific embodiment.
Water that the present invention applies is distilled water, medicine used has titanium isopropylate, tetrabutyl titanate, titanium tetrachloride, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH and TBAH, glacial acetic acid etc. are all provided by traditional Chinese medicines Reagent Company.
Embodiment 1
Under room temperature, magnetic agitation condition, by 20mL titanium isopropylate with in 10mL/ minute instillation 100mL distilled water, engender white precipitate.Separated by suction filtration method by white precipitate, filter cake is inserted distilled water again, stir after 20 minutes, then suction filtration is separated, this process repeats 3 times.After white product being mixed with 200mL water, adding 8mL concentration is the 25wt% TPAOH aqueous solution, stirs 2 hours.Above solution is transferred in 500mL static reaction still, after sealing, put into isothermal reaction in 80 DEG C of loft drier and, after 24 hours, add 4.5mL glacial acetic acid, rise oven temperature to 120 DEG C, isothermal reaction 24 hours.Take out reactor, after naturally cooling to room temperature, white powder is separated by centrifugal method.Three times are cleaned with distilled water, each centrifugal method isolates white powder, centrifugation rotating speed is 8000rpm, last 70 DEG C of dryings 24 hours, collect white powder, obtain product A, for transmission electron microscope observing and XRD analysis, the particle size of transmission electron microscope structure display titanium dioxide is about 20nm; XRD diffraction patterns display titanium dioxide is anatase structured.
Embodiment 2
By the process of embodiment 1, with TiCl
4for titanium precursors, TiCl
4add-on is 5mL, and sample processing conditions, with embodiment 1, obtains product B, and for transmission electron microscope observing and XRD analysis, the particle size of transmission electron microscope structure display titanium dioxide is about 20nm; XRD diffraction patterns display titanium dioxide is anatase structured.
Embodiment 3
By in 25mL tetrabutyl titanate instillation 120mL deionized water, form the precipitation of white, following process is identical with embodiment 1, and except hydrothermal treatment consists temperature is 140 DEG C, the reaction times is 12 hours.Obtain product C, for transmission electron microscope observing and XRD diffraction experiment, the size of transmission electron microscope results display titanium dioxide is about 15nm; XRD result display titanium dioxide is anatase structured.
Embodiment 4
By the process of embodiment 1, by in 10mL tetrabutyl titanate instillation 80mL deionized water, form the flocks of white, by 10mL concentration be 15wt% tetramethylammonium hydroxide aqueous solution with 20mL/ minute in above system, sample processing conditions is with embodiment 1, obtain product D, for transmission electron microscope observing and XRD diffraction experiment, the size of transmission electron microscope results display titanium dioxide is about 21nm; XRD result display titanium dioxide is anatase structured.
Embodiment 5
Under room temperature, magnetic agitation condition, by in 10mL titanium tetrachloride instillation 300mL deionized water, form the precipitation of white, after embodiment 1 process cleaning, be that the 40wt% TBAH aqueous solution is added drop-wise in above system with 50mL/ point of clock rate by 16mL concentration, above solution transferred in 500mL static reaction still, after sealing, after aging 24 hours, add 6mL glacial acetic acid at 90 DEG C, afterwards temperature is raised in 160 DEG C of loft drier and reacts 2 hours.Take out reactor, after naturally cooling to room temperature, white powder is separated by centrifugal method, and centrifugation rotating speed is 8000rpm.Sample processing conditions, with embodiment 1, obtains product E, and for transmission electron microscope observing and XRD diffraction experiment, the size of transmission electron microscope results display titanium dioxide is about 12nm; XRD result display titanium dioxide is anatase structured.
Comparative example 1
By 10mL tetrabutyl titanate and 60mL Virahol mixing, be made into A liquid, then the Virahol of 30mL and 10mL deionized water and 17mL tetraethyl ammonium hydroxide be made into B liquid.Under violent magnetic agitation condition, B liquid is slowly added drop-wise in A liquid, obtained homodisperse colloidal sol or gel.Then proceeded in the autoclave of teflon lined, constant temperature 8h in 200 DEG C of loft drier.The white depositions obtained with deionized water, acetone, dehydrated alcohol substep washing also centrifugation, obtains product F, uses transmission electron microscope observing pattern respectively.Result display is anatase structured titania nanoparticles, and nano particle is fusiformis, length about 100 nanometer, radial 20nm.
Comparative example 2
By 10mL tetrabutyl titanate and 10mL dehydrated alcohol and the mixing of 1ml glacial acetic acid, be made into solution A; Use 10ml dehydrated alcohol, 2mL glacial acetic acid and the mixing of 5mL distilled water, be made into B solution.Under strong magnetic agitation, solution A is instilled B solution, stir 3h, be aged to solution and lose flowability, 100 DEG C of dryings, dry, roasting 2 hours in 450 DEG C of retort furnaces after grinding, obtains product G.Result display structure is Detitanium-ore-type, but titanium dioxide pattern is random.
Comparative example 3
5mL tetrabutyl titanate is become clear solution with 50mL dehydrated alcohol, 5mL water is joined above solution, form white colloidal solution, the ammonium bicarbonate soln of 4 grams is joined in above colloidal solution, solution is transferred in reactor, be warmed up to 120 DEG C with 3 DEG C/min, isothermal reaction 6 hours.Solution separating after reacting, with washes of absolute alcohol three times, 50 DEG C of drying one nights.The product H obtained, the titanium dioxide size that result display obtains at 10 ~ 20nm, but still is reunited.
Comparative example 4
Adopt the experimentation identical with embodiment 1, but remove and add glacial acetic acid solution step.Obtain product I, result display titanium dioxide is random small-particle (10nm) and the mixing of macrobead (50nm).
Claims (10)
1. a synthetic method for nano-titanium dioxide powder, is characterized in that comprising the following steps: the presoma of titanium oxide is added drop-wise in water by (1), and be hydrolyzed reaction, generate white precipitate, white precipitate, through being separated, cleaning, is re-dispersed in water, obtains solidliquid mixture; (2) in the mixture of step (1), add alkyl phosphonium hydroxide ammonium solution, mix, aging; (3) add glacial acetic acid solution, isothermal reaction in step (2) ageing products, after reaction terminates, reaction product, through being separated, cleaning and drying, obtains nano-titanium dioxide powder.
2. in accordance with the method for claim 1, it is characterized in that: the titania precursor body described in step (1) is selected from one or more in titanium tetrachloride, titanium sulfate and Organic Alcohol oxygen titanium; Wherein Organic Alcohol oxygen titanium is one or more of titanium isopropylate, tetrabutyl titanate or titanium isopropylate.
3. in accordance with the method for claim 1, it is characterized in that: the dispersion described in step (1) is by H
2o/Ti mol ratio is 80 ~ 120, disperses with stirring or ultrasonic power.
4. in accordance with the method for claim 1, it is characterized in that: the mol ratio of the water described in step (1) and titanium is 10 ~ 100.
5. in accordance with the method for claim 1, it is characterized in that: the alkyl ammonium hydroxide described in step (2) is selected from one or more in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH or TBAH, the concentration of alkyl phosphonium hydroxide aqueous ammonium is 10wt% ~ 40wt%.
6. in accordance with the method for claim 1, it is characterized in that: the add-on of alkyl ammonium hydroxide described in step (2) with the mol ratio of ammonium and titanium for 0.3 ~ 0.7.
7. in accordance with the method for claim 1, it is characterized in that: the aging temperature described in step (2) is 50 ~ 90 DEG C, described digestion time is 10 ~ 30 hours.
8. in accordance with the method for claim 1, it is characterized in that: add glacial acetic acid amount described in step (3), is 0.5 ~ 2 by acetic acid/Ti mol ratio.
9. in accordance with the method for claim 1, it is characterized in that: the temperature of reaction described in step (3) is 120 ~ 220 DEG C of interval arbitrary temperature, and the described reaction times is 10 ~ 30 hours.
10. according to nanometer titanium dioxide titanium valve prepared by the method described in the arbitrary claim of claim 1 ~ 9, it is characterized in that: titanium dioxide has anatase structured, size range is 10-20nm, and specific surface area is 100 ~ 150m
2/ g, formed and pile up meso-hole structure, mesopore size is at 8-10nm.
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| CN106243680A (en) * | 2016-08-01 | 2016-12-21 | 江苏卧尔康家居用品有限公司 | A kind of nano titanium oxide strengthens the preparation method of polyurethane material |
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| CN109746021A (en) * | 2019-01-16 | 2019-05-14 | 浙江理工大学 | The preparation method and product of a kind of P-N hetero-junctions composite catalyst and application |
| CN113149147A (en) * | 2021-04-20 | 2021-07-23 | 昆明理工大学 | Doped nano TiO2Preparation method of photo-anode plate |
| CN114315885A (en) * | 2021-12-28 | 2022-04-12 | 山东金城柯瑞化学有限公司 | Method for catalytically synthesizing methyl 3-hydroxy-4- ((trimethylsilyl) ethynyl) benzoate |
| CN114315885B (en) * | 2021-12-28 | 2024-05-03 | 山东金城柯瑞化学有限公司 | Method for catalytic synthesis of methyl 3-hydroxy-4- ((trimethylsilyl) ethynyl) benzoate |
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