CN1323743A - Process of preparing titania sol from titanium tetrachloride - Google Patents
Process of preparing titania sol from titanium tetrachloride Download PDFInfo
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- CN1323743A CN1323743A CN 00110406 CN00110406A CN1323743A CN 1323743 A CN1323743 A CN 1323743A CN 00110406 CN00110406 CN 00110406 CN 00110406 A CN00110406 A CN 00110406A CN 1323743 A CN1323743 A CN 1323743A
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- Prior art keywords
- tio
- sol
- titanium tetrachloride
- prepare
- colloidal sol
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- 238000000034 method Methods 0.000 title claims abstract description 23
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract description 16
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 26
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000010936 titanium Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000012670 alkaline solution Substances 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 19
- 238000009826 distribution Methods 0.000 abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000843 powder Substances 0.000 abstract description 5
- 239000002244 precipitate Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 4
- 229910003074 TiCl4 Inorganic materials 0.000 abstract 1
- 239000003513 alkali Substances 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- -1 titanium alkoxide Chemical class 0.000 abstract 1
- 239000004408 titanium dioxide Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 11
- 239000012071 phase Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 150000004703 alkoxides Chemical class 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
一种由四氯化钛制备二氧化钛溶胶方法,其特征在于:以TiCl4为原料与碱溶液作用生成沉淀,pH=6～7,此沉淀经洗涤后,加入水和酸溶液,加酸量为[H+]/[Ti]摩尔比为0.2～1.0,在0～90℃下搅拌,解胶12～60小时后,得到稳定的TiO2溶胶。本发明制备得到的TiO2溶胶稳定,粒度分布均一,溶胶粒径可通过调节酸浓度等制备因素得以控制,由此法制备的TiO2溶胶及其由它得到的TiO2粉体的性质与由钛醇盐制备得到的TiO2溶胶及粉体的性质相似。该方法成本低廉,易于大规模生产。A method for preparing titanium dioxide sol from titanium tetrachloride, which is characterized in that: TiCl4 is used as a raw material to interact with an alkali solution to form a precipitate, pH = 6-7, after the precipitate is washed, water and an acid solution are added, and the amount of acid added is The [H + ]/[Ti] molar ratio is 0.2-1.0, stirring at 0-90°C, and degelling for 12-60 hours to obtain a stable TiO 2 sol. The TiO2 sol prepared by the present invention is stable, has a uniform particle size distribution, and the particle size of the sol can be controlled by adjusting the preparation factors such as acid concentration. The properties of the TiO2 sol prepared by this method and the TiO2 powder obtained by it are similar to The properties of TiO 2 sol and powder prepared by titanium alkoxide are similar. This method is cheap and easy to produce on a large scale.
Description
The present invention relates to the preparation of the preparation of nano material, particularly nano titanium oxide.
Nano-TiO
2Be a kind of catalysis that is widely used in, absorption, transmitter, makeup, sensitive materials, ceramic additive, the high function fine inorganic material in fields such as electronic engineering, especially TiO
2The film coating material have prior using value in these fields.At present, synthesis of nano TiO
2Method mainly be traditional sol-gel method (sol～gel) and vapor phase process (CVD).Utilizing the hydrolysis of metal alkoxide and the sol-gel method of polycondensation is a kind of effective ways that prepare nano material, has synthesized the TiO of size-grade distribution homogeneous
2Colloidal sol and nano-TiO
2Powder, but metal alkoxide costs an arm and a leg, toxicity is big, and facile hydrolysis is inflammable, is unfavorable for scale operation.And the CVD rule requires height aspect technology and material, complex process, and investment is big.Therefore, develop a kind of with low costly, simple to operate, be easy to the TiO of scale operation
2The preparation method of colloidal sol is very necessary, and it more helps further developing nano-TiO
2Material and relevant TiO
2Material elements.
The object of the present invention is to provide a kind of preparation method of TiO 2 sol, this method cost of material is cheap, prepared colloidal sol is stable, little and the homogeneous of granularity, in the properties of colloidal sol and formed material thereof and traditional by the colloidal sol of metal alkoxide preparation and the similar performance of respective material, and simple to operate, be easy to scale operation.
The invention provides and a kind ofly prepare TiO 2 sol, it is characterized in that: with TiCl by titanium tetrachloride
4Be raw material, generate precipitation with the alkaline solution effect, pH=6～7, this precipitation adds entry and acid solution after washing, add the acid amount and be [H
+]/[Ti] mol ratio is 0.2～1.0, stirs down at 0～90 ℃, dispergation obtained stable TiO after 12～60 hours
2Colloidal sol.
The alkaline solution that adopts in preparation method of the present invention is selected from ammoniacal liquor, urea, and NaOH, KOH etc. wherein are best with ammoniacal liquor, ammonia concn is advisable 7～10%.Because ammoniacal liquor is a kind of weak base, with TiCl
4When effect generates precipitation, can reduce generating sedimentary speed, make the precipitation granularity of generation little and even, be more conducive to next step dispergation, ammoniacal liquor can decompose fully at a certain temperature in addition, can residual other ion and influence TiO after the colloidal sol moulding thus
2The character of material.The acid of being adopted is mineral acid, as HCl, and HNO
3, H
2SO
4Deng, wherein with HCl, HNO
3Be the best.Acidity i.e. [H
+]/[Ti] mol ratio be the preparation in of paramount importance factor, by the allotment [H
+]/[Ti] mol ratio can control the size-grade distribution of colloidal sol, [H
+]/[Ti] scope of mol ratio is generally 0.2～1.0, [H wherein
+]/[Ti]=0.4～0.6 o'clock the preparation colloidal sol median size minimum, it is the narrowest, the most stable to distribute, and can keep some months.The preparation temperature scope is 0～90 ℃, and is wherein suitable with 60～80 ℃.
Give further instruction below by embodiment to preparation method provided by the invention.
Accompanying drawing 1 TiO
2Size-grade distribution (the H of colloidal sol
+/ Al=0.5)
The XRD spectra of accompanying drawing 2 sample after treatment of different temperature (● Detitanium-ore-type TiO
2, the rutile TiO
2, NH
4Cl)
The graph of pore diameter distribution of accompanying drawing 3 sample after 450 ℃ of roastings
Accompanying drawing 4 different pH values are [PtCl down
4]
2-Ion is at TiO
2On adsorption curve
Example 1.TiO
2The preparation of colloidal sol.
Take by weighing 11.4 gram TiCl
4Place separating funnel, after dropwise joining in the HCl solution of 25ml37%, dropwise add the 70ml secondary deionized water again, after stirring half an hour, drip 7%～10% ammoniacal liquor again and o'clock generate white precipitate to pH=6～7, aging one hour, filter, wash (each wash agitation is half an hour approximately) to there not being Cl with 40～50 ℃ of secondary deionized water
-Ion.Then this throw out is joined in the secondary deionized water of 200ml, add the HNO of a certain amount of 1.6M
3Solution, 70 ℃ were stirred dispergation 48 hours down, promptly obtain the TiO of size-grade distribution homogeneous
2Colloidal sol.Drying is 24 hours under 50 ℃, and roasting obtained TiO after 3 hours under the certain temperature
2Powder.
Example 2. acidity are to TiO
2The influence of colloidal sol granularity.
Utilize the above-mentioned colloidal sol of transmission electron microscope observing, can find that their micelle all is spherical.Table 1 has been listed different [H
+]/[Ti] TiO under the mol ratio
2The size-grade distribution of colloidal sol.Data show the stability that can control the particle diameter and the colloidal sol of colloidal sol by the concentration of regulating acid, work as H
+/ Ti mol ratio is the median size minimum of colloidal sol of preparation in 0.5 o'clock, and size-grade distribution is the narrowest, and colloidal sol is also the most stable, can place the several months not precipitate or gelling, and the size-grade distribution of this colloidal sol as shown in Figure 1.Table 1 acid concentration is to TiO
2The influence of colloidal sol particle diameter.
| Sample | TiO 2Collosol concentration (M) | H +/ Ti (mol ratio) | Median size (nm) | Collosol stability |
| ????T1 ????T2 ????T3 ????T4 ????T5 ????T6 ????T7 | 0.3125 0.3125 0.3125 0.3125 0.3125 0.3125 0.3125 | 0.08 0.2 0.4 0.5 0.7 1.0 1.2 | ?- 102 45 14 56 96 - | Can not the stable instability of dispergation |
Example 3. crystalline phase analyses.
With X-ray diffraction (XRD) to studying, to understand the variation of crystalline phase in roasting process through differing temps agglomerating sample.Accompanying drawing 2 is without roasting and the XRD spectra after the differing temps roasting behind the example 1 preparation colloidal sol sample drying.Can find to have weak anatase phase, but have tangible NH therein without heat treated gel sample
4The Cl crystalline phase, this be since in this method in order to regulate the ammoniacal liquor and the raw material TiCl of pH value
4In Cl
-Ion generates NH
4Due to the Cl.NH after 450 ℃ of burnings
4The Cl crystalline phase disappears, and shows as Detitanium-ore-type, is the mixed phase of anatase octahedrite and rutile after 600 ℃ of roastings.
Example 4. differential thermals and thermogravimetric analysis
The TiO of this method preparation will be utilized
2The dried sample of colloidal sol carries out heat analysis.As can be seen, from room temperature to 800 two variations ℃ have taken place from its differential thermal curve: room temperature-220 ℃ still is the evaporation of water the gel network, and 260-450 ℃ then is NH
4The decomposition peak of Cl, NH
4Also not having tangible thermal phenomenon the crystalline phase of Cl has been found that 450 ℃ in XRD analysis after takes place.
Example 5. pore structure parameters
Surface-area, aperture and pore size distribution are the important structural parameter of catalytic material.We study the TiO of this method preparation with low-temperature nitrogen adsorption method
2Colloidal sol is dry after the surface-area of the sample of 450 ℃ of roastings and pore structure.Its surface-area is 74.7m
2/ g, pore volume are 0.11ml/g.Accompanying drawing 3 has shown its pore size distribution respectively.Can find that this sample has single pore distribution, its most probable aperture is about about 4.6nm.By they adsorption isothermal line as can be known, be a mesopore material.
The comparative example alkoxide hydrolysis prepares TiO
2Colloidal sol
Get the mixing solutions of certain density titanium isopropylate and Virahol, be added drop-wise in the secondary deionized water of certain volume under 30 ℃, form white precipitate, add an amount of 1.6M salpeter solution, make H
+/ Ti mol ratio is 0.4,30 ℃ of following dispergation 48 hours, obtains stable sols.After this drying sol roasting, the drying and roasting process is described identical with example 1, carries out XRD, differential thermal, and thermogravimetric, analyses such as cryogenic nitrogen absorption are with the TiO that utilizes method preparation in this patent
2Sample relatively finds to utilize the colloidal sol of present method preparation and character and the colloidal sol of alkoxide hydrolysis preparation and the similar performance of material of powder body material thereof.
Claims (6)
1, a kind ofly prepares the TiO 2 sol method, it is characterized in that: with TiCl by titanium tetrachloride
4Be raw material, generate precipitation with the alkaline solution effect, pH=6～7, this precipitation adds entry and acid solution after washing, add the acid amount and be [H
+]/[Ti] mol ratio is 0.2～1.0, stirs down at 0～90 ℃, dispergation obtained stable TiO after 12～60 hours
2Colloidal sol.
2, prepare the TiO 2 sol method according to claim 1 is described by titanium tetrachloride, it is characterized in that: [H
+]/[Ti] mol ratio is 0.4～0.6.
3, prepare the TiO 2 sol method according to claim 1 is described by titanium tetrachloride, it is characterized in that: 60～80 ℃ of dispergation temperature.
4, prepare the TiO 2 sol method according to claim 1 is described by titanium tetrachloride, it is characterized in that: be used for and TiCl
4Effect generates sedimentary alkaline solution and selects the weak base of ammoniacal liquor, urea or the lower concentration strong base solution of rare NaOH, KOH for use.
5. prepare the TiO 2 sol method according to claim 4 is described by titanium tetrachloride, it is characterized in that: alkaline solution is selected ammoniacal liquor for use, and concentration is 7～10%.
6, describedly prepare the TiO 2 sol method according to claim 1 or 2, it is characterized in that: be used for the sedimentary acid solution of dispergation and select HCl for use, HNO by titanium tetrachloride
3Inorganic acid solution.
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|---|---|---|---|
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|---|---|---|---|
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|---|---|---|---|
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1300001C (en) * | 2004-12-24 | 2007-02-14 | 广东省生态环境与土壤研究所 | Preparation method of visible light photoactivated octahedrite type titanium oxide colloidal sols |
| CN1313204C (en) * | 2004-10-13 | 2007-05-02 | 河南工业大学 | Process for preparing nanometer titania doping photocatalyst |
| CN1315731C (en) * | 2002-03-01 | 2007-05-16 | 徐瑞芬 | Method of controlling nano titanium dioxide crystal form and obtained nano titanium dioxide using said method |
| CN1325577C (en) * | 2004-12-03 | 2007-07-11 | 中国科学院长春应用化学研究所 | Process for synthesizing organic ligand coated titanium dioxide nano particles |
| CN100337740C (en) * | 2004-06-15 | 2007-09-19 | 刘文泉 | Crystalline titanium dioxide photocatalyst and its synthesis method |
| CN100431813C (en) * | 2004-05-31 | 2008-11-12 | 丽水市吉丽斯纺织材料有限公司 | Nano pulp composition and its preparation method |
| CN102786087A (en) * | 2012-08-22 | 2012-11-21 | 厦门大学 | Method for preparing titanium dioxide sol |
| CN104448962A (en) * | 2014-12-29 | 2015-03-25 | 连云港职业技术学院 | Self-cleaning nano-oxide coating material preparation method |
| CN105935552A (en) * | 2016-04-30 | 2016-09-14 | 安吉云界生物科技有限公司 | Road additive having automobile tail gas degradation function and preparation method thereof |
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-
2000
- 2000-05-12 CN CN 00110406 patent/CN1323743A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1315731C (en) * | 2002-03-01 | 2007-05-16 | 徐瑞芬 | Method of controlling nano titanium dioxide crystal form and obtained nano titanium dioxide using said method |
| CN100431813C (en) * | 2004-05-31 | 2008-11-12 | 丽水市吉丽斯纺织材料有限公司 | Nano pulp composition and its preparation method |
| CN100337740C (en) * | 2004-06-15 | 2007-09-19 | 刘文泉 | Crystalline titanium dioxide photocatalyst and its synthesis method |
| CN1313204C (en) * | 2004-10-13 | 2007-05-02 | 河南工业大学 | Process for preparing nanometer titania doping photocatalyst |
| CN1325577C (en) * | 2004-12-03 | 2007-07-11 | 中国科学院长春应用化学研究所 | Process for synthesizing organic ligand coated titanium dioxide nano particles |
| CN1300001C (en) * | 2004-12-24 | 2007-02-14 | 广东省生态环境与土壤研究所 | Preparation method of visible light photoactivated octahedrite type titanium oxide colloidal sols |
| CN102786087A (en) * | 2012-08-22 | 2012-11-21 | 厦门大学 | Method for preparing titanium dioxide sol |
| CN104448962A (en) * | 2014-12-29 | 2015-03-25 | 连云港职业技术学院 | Self-cleaning nano-oxide coating material preparation method |
| CN105935552A (en) * | 2016-04-30 | 2016-09-14 | 安吉云界生物科技有限公司 | Road additive having automobile tail gas degradation function and preparation method thereof |
| CN108298580A (en) * | 2018-05-04 | 2018-07-20 | 福建贝思科电子材料股份有限公司 | A kind of colloidal tio 2 and preparation method thereof |
| CN108298580B (en) * | 2018-05-04 | 2019-03-05 | 福建贝思科电子材料股份有限公司 | A kind of colloidal tio 2 and preparation method thereof |
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