CN1384151A - Prepn process of optically active enclosed nano-level titania functional stuffing - Google Patents
Prepn process of optically active enclosed nano-level titania functional stuffing Download PDFInfo
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- CN1384151A CN1384151A CN 01112819 CN01112819A CN1384151A CN 1384151 A CN1384151 A CN 1384151A CN 01112819 CN01112819 CN 01112819 CN 01112819 A CN01112819 A CN 01112819A CN 1384151 A CN1384151 A CN 1384151A
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Abstract
The present invention relates to a preparation process of optically active enclosed nanometer-level titania functional stuffing. metatitanic acid as main raw material is mixed with special additive for controlling the crystal structure of titania to obtain hydrated titania with rutile phase structure; the hydrated titania is then calcined to obtain nanometer-level TiO2 particle; and the nanometer-level TiO2 particle is optically active enclosed and functional treated through a special technological process to obtain the optically active enclosed nanometer-level TiO2 functional stuffing. The stuffing has high visibiel high transmittance and high ultraviolet light shielding performance and thus wide application foreground.
Description
The present invention relates to a kind of method for preparing titania functional stuffing, relate in particular to a kind of method for preparing optically active enclosed nano-level titania functional stuffing.
The nanoparticle size is greater than cluster, and the particulate less than common is generally 1～100nm.Nanoparticle has shell structure, and the particle surface atom accounts for significant proportion and is the unordered vaporous structure of class, then exists in particle inside in order-disordered structure.This singularity that is different from body phase sample has caused it and the solid that constitutes thereof to have small-size effect (volume effect), surface and interfacial effect, quantum size effect and macro quanta tunnel effect.Thereby make nanoparticle compare physics, chemical property such as having a series of new optics, catalysis, chemical reaction with conventional powder body material, all having a wide range of applications aspect catalysis, magneticsubstance, transmitter, medical science, the biotechnology.
Titanium dioxide is a kind of and the very close important industrial chemicals of modern life relation, is one of chemical industry pillar.Nano-titanium oxide can see through visible light and scattering and absorption UV-light, is good ultravioletlight screening material; This material also can prepare changeable colors along with angle coating with the effect pigment compatibility, makes coating produce abundant and Magic color.Rutile type nano TiO wherein
2Particle physics, chemical stability, and weathering resistance etc. all is better than the anatase titanium dioxide particle.Nano-titanium oxide has shown wide application prospect in fields such as packaging material for food, high-grade printing ink paint, plastics, catalyzer raw material, absorption agent, fine ceramics.Titanium dioxide has certain photocatalytic under illumination, make polymeric substrate produce to a certain degree oxidative degradation, thereby influences the work-ing life of material.The nano titanium dioxide photocatalysis activity depends on the form of product to a great extent, and particle shape and technology of preparing, method of modifying are closely related.
Produce the Nano titanium dioxide particle the whole bag of tricks is arranged.For example in Chinese patent CN1114949A, just described and utilized ilmenite and technical hydrochloric acid to be raw material, prepared the Nano titanium dioxide particle by steps such as organic substance extraction, ordinary-pressure hydrolysis; United States Patent (USP) 5840111 has proposed to adopt organic titanic compound to prepare the method for superfine TiO 2 particles through sol-gel; Shi Liyi etc. have also proposed preparation and have improved stable titaniferous ionogen microemulsion, the technology (functional materials, 1999 the 5th phases) of preparation titanium dioxide ultra-fine grain in microemulsion water nuclear.The shortcoming of these methods is that raw materials cost height, production efficiency are low, and at first obtains unformed hydrated titanium dioxide in the preparation process, needs could obtain rutile titanium dioxide through high temperature (～900 ℃) calcining, and the calcination process process very easily causes the particle sintering to be grown up.Shi Liyi etc. describe the method that the aerosol reaction method prepares the technology (material Leader, 1998 the 2nd phases) of Nano titanium dioxide and aluminium titania type nano titanium oxide is mixed in employing in the High Temperature Gas phase reactor that adopts in detail.The High Temperature Gas phase reaction is very high to the requirement of device structure, material and operation.It is raw material that CN11192992 provides with the metatitanic acid, use the method for Preparation by Uniform Precipitation superfine TiO 2 particles, this method reactant concn in building-up process is very low, influence production efficiency, and this patent lacks the method for effectively regulating the titanium dioxide crystal form structure, still needs to obtain the rutile titanium dioxide particle by high-temperature calcination; EP444982 adds water again and makes slurry by the hydrated titanium dioxide that hydrolytic action obtained of titanyl sulfate solution, and heating is added to it in sodium hydroxide solution of heat then.The mixture that is produced is kept for some time under boiling temperature.At this moment, the suspension that contains sodium titanate adds hydrochloric acid again and makes the mixture peptization through cooling, filtration, make tiny rutile phase hydrated titanium dioxide particle, but this particle still has stronger photocatalytic activity, the organic substrate that destructible contacts with it.CN1064285 provides a kind of adding SnO
2Crystal seed prepares the method for rutile type nano titanic oxide, but SnO
2Can increase substantially the titanium dioxide photolytic activity after mixing, and the time preparation SnO that implements this method
2Crystal seed is difficulty very, the too short or oversize effect that all can not effectively bring into play crystal seed storage period of preparation time, and what obtain still is the mixed type hydrated titanium dioxide.US5451252 provides a kind of doping zinc, antimony, iron plasma to eliminate the photoactive method of titanium dioxide, but dopant ion influences product purity, and easily make titanium dioxide painted, be difficult to obtain pure white titania nanoparticles, dopant ion that has such as zinc can cause the titanium dioxide crystal form structure to change, the hydrated titanium dioxide that obtains need obtain rutile titanium dioxide by high-temperature calcination for mixing crystal formation.CN1161307A provides a kind of technology of utilizing the rutile titanium dioxide crystal seed to prepare submicron order coating titanium white, the hydrated titanium dioxide of this method preparation still mainly is sharp titanium phase structure, thereby still need high-temperature calcination to prepare rutile titanium dioxide, the particle that obtains is 0.2～0.3 μ m, is difficult to obtain Nano titanium dioxide.Loss of gloss, variable color, efflorescence and the peeling phenomenon of the coating that causes for the photocatalysis characteristic that overcomes owing to titanium dioxide, EP393857 provides a kind of submicron order (0.2～0.3 μ m) coating level titanium white surface to coat the technology of silicon oxide treatment agent, can improve titanium oxide opacifying power and weathering resistance, handle but this method mainly is applicable to the submicron order titanium dioxide surface.
Purpose of the present invention be exactly provide in order to overcome the defective that above-mentioned prior art exists a kind of technology simple, be easy to control, the method for nano-level titania functional stuffing that lower-cost preparation is optically active enclosed.
Purpose of the present invention can be achieved through the following technical solutions: a kind of method for preparing the optically active enclosed meter level titania functional stuffing of receiving, be characterized in, metatitanic acid during with the Production By Sulfuric Acid Process titanium white is a raw material, and concrete processing step is as follows: the first step, at first prepare TiO
2Content is the metatitanic acid suspension of 20g/l～40g/l, add 40～50% (weight) sodium hydroxide solutions and a certain amount of rutile titanium dioxide crystal seed colloidal sol that contains, be warming up to 90 ℃～100 ℃ reactions 1～2 hour, cooling, filtration, filter cake adds hydrochloric acid and sizes mixing, heat treated 1～2 hour, cold filtration, washing are to using AgNO then
3Detect no Cl
-, calcined 1.5～2 hours down at 300 ℃～600 ℃, get nm-class rutile-type TiO
2Particle; Second step is with nm-class rutile-type TiO
2Particle adds certain amount of surfactant after adding water to concentration 200g/l～300g/l, after disperseing, sand milling adds a certain amount of sodium silicate solution, be warming up to 70 ℃～90 ℃, adding acid for adjusting pH value is 6.0～8.0, slaking 1～2 hour, filtration drying obtains optically active enclosed nano-level titania functional stuffing.
The described preparation method who contains rutile titanium dioxide crystal seed colloidal sol is: in 110g/l NaOH solution, add 50% (weight) TiCl
4Solution, NaOH solution and TiCl
4The liquor capacity ratio is 3: 1, is warming up to 900 ℃, and isothermal reaction adds the cold water dilution after 1～2 hour, and being adjusted to the pH value with NaOH solution is 7～8.5, and wherein content of titanium dioxide is 16g/l.
Described TiCl
4Solution is TiCl
4Hydrochloric acid soln, the concentration of its hydrochloric acid soln are 35% (weight).
The add-on of described rutile titanium dioxide crystal seed colloidal sol be that titanium dioxide accounts for prepared titania functional stuffing weight in the crystal seed 1～5%.
Described tensio-active agent is an xylonic acid sodium, and add-on is 0.005～0.01% of a prepared titania functional stuffing weight.
The content of silicon oxide is 100g/l in the described sodium silicate solution, and the add-on of sodium silicate solution is 5～15% of the covering amount of the silicon oxide titania functional stuffing weight that accounts for preparation.
Compared with prior art, the present invention's advantage of giving prominence to is:
1) containing the rutile titanium dioxide crystal seed can be now with the current, very convenient.
2) adopt specific nano titanium oxide surface to coat the silicon oxide technology, can form uniform silicon oxide coating layer on the nano titanium oxide surface, this coating layer not only can seal the photocatalytic activity of nano titanium oxide, can also produce synergistic effect with titanium oxide, improve the particle transparency and shielding ultraviolet rays ability.
3) preparation process provided by the invention is simple and easy to control, is liquid phase reaction under the normal pressure, easily expands commercial scale production to.
4) constant product quality, outward appearance are extremely white, and wherein titanium dioxide is the rutile phase structure, particle size distribution 20～40nm.
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail.
Fig. 1 obtains the XRD spectra of hydrated titanium dioxide for embodiment 1;
Fig. 2 obtains calcining the XRD spectra of back product for embodiment 1;
Fig. 3 obtains the UV-Vis spectrogram of product for embodiment 1,2,3;
Fig. 4 obtains the TEM spectrogram of product for embodiment 1.
The present invention has disclosed and has been used for a kind of of optically active enclosed rutile type nano titanic oxide functional stuffing production New technology, it has overcome the defective of existing production method, and the Nano titanium dioxide of producing has extremely low light Catalytic activity has the excellent transparency and ultraviolet screener ability. The characteristics of this new technology are to produce two During titanium oxide, adding quantity is to tie with respect to the Rutile Type of prepared titanium dioxide amount 1～5% percentage by weight The titanium dioxide crystal seed of structure obtains the Rutile Type hydrated titanium dioxide through reaction, through calcining preparation nanoscale two Titanium oxide. The nano-scale particle surface energy is very big, very easily produces between particle and reunites. The invention provides a kind of specific Titanium dioxide nanoparticle disperse and the coating means, in a certain amount of oxidation of nano titanium oxide coated with uniform Silicon, silica addition are with respect to 5～15% of prepared titanium dioxide amount, are preferably about 10% this oxygen The SiClx clad can also produce association with titanium dioxide except effectively sealing the nano titanium dioxide photocatalysis activity Same effect improves particle ultraviolet screener ability.
It is that the Rutile Type structure (adopts that the present invention prepares in the nano-level titania functional stuffing titanium dioxide composition The XRD test), the titania size is determined according to XRD broadening experiment employing Scherre formula. Dioxy SiClx is undefined structure, and particle size distribution is 20～40nm (employing tem observation). Photocatalytic activity Evaluation method be: take by weighing the dyestuff acid red of 0.02g, the dissolving be placed in the volumetric flask of 1000ml, add water To scale, concussion shakes up, and is made into the dye solution that concentration is 20mg/l; Get above-mentioned dye solution 250ml, The pH=2.5 of regulator solution surveys initial absorbance A0; In dye solution, add 0.2g nano particle sample, Stir, (wavelength 200～250nm) carries out light-catalyzed reaction, liquid level and light as light source take the 8W uviol lamp The distance in source is 17 centimetres, passes into air from reactor bottom with 0.14m3/h speed. According to reaction 60min Rear dyestuff percent of decolourization is weighed catalyst activity. When X-3B concentration during less than 70mg/L, reactive red solution is The absorptance A at big absorbing wavelength 510nm place and concentration C Relations Among are observed Lang Bai-law of Beer, namely A=ε bC, then Decoloration Experiments of Vital Red rate η=(A0-A)/A0. Concrete grammar is: extract 5～10ml behind the reaction 60min Reactant liquor through 16000 rev/mins of lower centrifugal 10min, is got clear liquid and is adopted 7230 spectrophotometric determination solution Absorbance, thus dye decolored rate calculated. Nano particle is mixed with 0.02% aqueous solution, adopts ultraviolet-visible Spectrophotometer particle tested optical characteristics.
Embodiment 1
Get 77g and be the metatitanic acid of anatase octahedrite phase structure after washing, it is the formed titanyl sulfate solution of ilmenite boiling in sulfuric acid, separates ferrous sulfate after the hydrolysis and gets, and thin up is to TiO
2Content 30g/l adds 40% sodium hydroxide solution and the colloidal sol that contains the rutile titanium dioxide crystal seed, and the titanium dioxide amount is 5% of a prepared titania functional stuffing weight in the colloidal sol, is warming up to 100 ℃ of reactions 2 hours, cooling, filtration; Filter cake adds 10% hydrochloric acid soln sizes mixing, to TiO
2Content 30g/l, 80 ℃ of reactions 2 hours, cold filtration, washing were to using AgNO then
3Detect no Cl
-, filtration cakes torrefaction must be had the hydrated titanium dioxide (see figure 1) of rutile phase structure, through 600 ℃ of calcinings 2 hours, nm-class rutile-type TiO
2Particle (see figure 2), average grain size are 12nm, and this particle photocatalytic degradation of dye percent of decolourization is about 12.8%, and its optical characteristics is seen curve a and b among Fig. 3; Nm-class rutile-type TiO with gained
2Particle adds the water making beating, suspension concentration is 300g/l, add 0.01% xylonic acid sodium, sand milling adds sodium silicate solution (silica content is 100g/l) after 2 hours, the silicon oxide amount is 10% of a nano titanium oxide weight, is warming up to 90 ℃, adding dilute sulphuric acid adjusting pH of suspension value is 8.5, slaking reaction 2 hours gets nano-level titania functional stuffing after filtration, drying, the pulverizing, and particle diameter is 20～40nm (see figure 4).This particle photocatalytic degradation of dye percent of decolourization is 2.4%, and photocatalytic activity is effectively sealed.Its optical characteristics is seen curve c and d among Fig. 3, and this particle shielding ultraviolet rays ability is strong, and has the transparency preferably at visible region.
The preparation method of above-mentioned rutile titanium dioxide crystal seed colloidal sol is: in a certain amount of 110g/l NaOH solution, add 50%TiCl
4Hydrochloric acid (35%) solution, NaOH solution and TiCl
4The liquor capacity ratio is 3: 1, is warming up to 900C, and isothermal reaction adds a certain amount of cold water after 2 hours, and being adjusted to the pH value with NaOH solution is 7～8.5, and wherein content of titanium dioxide is 16g/l.
Embodiment 2
Get 77g and be the metatitanic acid of anatase octahedrite phase structure after washing, it is the formed titanyl sulfate solution of ilmenite boiling in sulfuric acid, separates ferrous sulfate after the hydrolysis and gets, and thin up is to TiO
2Content 20g/l adds 40% sodium hydroxide solution and the colloidal sol that contains the rutile titanium dioxide crystal seed, and the titanium dioxide amount is 5% of a prepared titania functional stuffing weight in the colloidal sol, is warming up to 100 ℃ of reactions 1 hour, cooling, filtration; Filter cake adds 10% hydrochloric acid soln sizes mixing, to TiO
2Content 30g/l, 80 ℃ of reactions 2 hours, cold filtration, washing were to using AgNO then
3Detect no Cl
-, the hydrated titanium dioxide with filtration cakes torrefaction must have the rutile phase structure through 300 ℃ of calcinings 2 hours, gets nm-class rutile-type TiO
2Particle, average grain size are 12nm, and this particle photocatalytic degradation of dye percent of decolourization is about 12.8%, and its optical characteristics is seen curve a and b among Fig. 3; Nm-class rutile-type TiO with gained
2Particle adds the water making beating, suspension concentration is 200g/l, add 0.005% xylonic acid sodium, sand milling adds sodium silicate solution (silica content is 100g/l) after 2 hours, the silicon oxide amount is 10% of a nano titanium oxide weight, is warming up to 70 ℃, adding dilute sulphuric acid adjusting pH of suspension value is 6, slaking reaction 1 hour gets nano-level titania functional stuffing after filtration, drying, the pulverizing, and particle diameter is 20～40nm.This particle photocatalytic degradation of dye percent of decolourization is 3%, and photocatalytic activity is effectively sealed.Its optical characteristics is seen curve c and d among Fig. 3, and this particle shielding ultraviolet rays ability is stronger, and has the transparency preferably at visible region.
The preparation method of above-mentioned rutile titanium dioxide crystal seed colloidal sol is: in a certain amount of 110g/l NaOH solution, add 50%TiCl
4Hydrochloric acid (35%) solution, NaOH solution and TiCl
4The liquor capacity ratio is 3: 1, is warming up to 900C, and isothermal reaction adds a certain amount of cold water after 2 hours, and being adjusted to the pH value with NaOH solution is 7～8.5, and wherein content of titanium dioxide is 16g/l.
Embodiment 3
Get 77g and be the metatitanic acid of anatase octahedrite phase structure after washing, it is the formed titanyl sulfate solution of ilmenite boiling in sulfuric acid, separates ferrous sulfate after the hydrolysis and gets, and thin up is to TiO
2Content 40g/l adds 50% sodium hydroxide solution and the colloidal sol that contains the rutile titanium dioxide crystal seed, and the titanium dioxide amount is 5% of a prepared titania functional stuffing weight in the colloidal sol, is warming up to 100 ℃ of reactions 2 hours, cooling, filtration; Filter cake adds 10% hydrochloric acid soln sizes mixing, to TiO
2Content 30g/l, 80 ℃ of reactions 1 hour, cold filtration, washing were to using AgNO then
3Detect no Cl
-, the hydrated titanium dioxide with filtration cakes torrefaction must have the rutile phase structure through 500 ℃ of calcinings 2 hours, gets nm-class rutile-type TiO
2Particle, average grain size are 12nm, and this particle photocatalytic degradation of dye percent of decolourization is about 12.8%, and its optical characteristics is seen curve a and b among Fig. 3; Nm-class rutile-type TiO with gained
2Particle adds the water making beating, suspension concentration is 300g/l, add 0.01% xylonic acid sodium, sand milling adds sodium silicate solution (silica content is 100g/l) after 2 hours, the silicon oxide amount is 10% of a nano titanium oxide weight, is warming up to 90 ℃, adding dilute sulphuric acid adjusting pH of suspension value is 8, slaking reaction 2 hours gets nano-level titania functional stuffing after filtration, drying, the pulverizing, and particle diameter is 20～40nm.This particle photocatalytic degradation of dye percent of decolourization is 2.4%, and photocatalytic activity is effectively sealed.Its optical characteristics is seen curve c and d among Fig. 3, and this particle shielding ultraviolet rays ability is strong, and has the transparency preferably at visible region.
The preparation method of above-mentioned rutile titanium dioxide crystal seed colloidal sol is: in a certain amount of 110g/l NaOH solution, add 50%TiCl
4Hydrochloric acid (35%) solution, NaOH solution and TiCl
4The liquor capacity ratio is 3: 1, is warming up to 900C, and isothermal reaction adds a certain amount of cold water after 2 hours, and being adjusted to the pH value with NaOH solution is 7～8.5, and wherein content of titanium dioxide is 16g/l.
Claims (6)
1. a method for preparing optically active enclosed nano-level titania functional stuffing is characterized in that, the metatitanic acid during with the Production By Sulfuric Acid Process titanium white is a raw material, and concrete processing step is as follows: the first step, at first prepare TiO
2Content is the metatitanic acid suspension of 20g/l～40g/l, add 40～50% (weight) sodium hydroxide solutions and a certain amount of rutile titanium dioxide crystal seed colloidal sol that contains, be warming up to 90 ℃～100 ℃ reactions 1～2 hour, cooling, filtration, filter cake adds hydrochloric acid and sizes mixing, heat treated 1～2 hour, cold filtration, washing are to using AgNO then
3Detect no Cl
-, calcined 1.5～2 hours down at 300 ℃～600 ℃, get nm-class rutile-type TiO
2Particle; Second step is with nm-class rutile-type TiO
2Particle adds certain amount of surfactant after adding water to concentration 200g/l～300g/l, after disperseing, sand milling adds a certain amount of sodium silicate solution, be warming up to 70 ℃～90 ℃, adding acid for adjusting pH value is 6.0～8.0, slaking 1～2 hour, filtration drying obtains optically active enclosed nano-level titania functional stuffing.
2. the method for the nano-level titania functional stuffing that preparation as claimed in claim 1 is optically active enclosed, it is characterized in that, the described preparation method who contains rutile titanium dioxide crystal seed colloidal sol is: in 110g/l NaOH solution, add 50% (weight) TiCl
4Solution, NaOH solution and TiCl
4The liquor capacity ratio is 3: 1, is warming up to 900 ℃, and isothermal reaction adds the cold water dilution after 1～2 hour, and being adjusted to the pH value with NaOH solution is 7～8.5, and wherein content of titanium dioxide is 16g/l.
3. the method for the nano-level titania functional stuffing that preparation as claimed in claim 2 is optically active enclosed is characterized in that, described TiCl
4Solution is TiCl
4Hydrochloric acid soln, the concentration of its hydrochloric acid soln are 35% (weight).
4. the method for the nano-level titania functional stuffing that preparation as claimed in claim 1 is optically active enclosed, it is characterized in that, the add-on of described rutile titanium dioxide crystal seed colloidal sol be that titanium dioxide accounts for prepared titania functional stuffing weight in the crystal seed 1～5%.
5. the method for the nano-level titania functional stuffing that preparation as claimed in claim 1 is optically active enclosed is characterized in that, described tensio-active agent is an xylonic acid sodium, and add-on is 0.005～0.01% of a prepared titania functional stuffing weight.
6. the method for the nano-level titania functional stuffing that preparation as claimed in claim 1 is optically active enclosed, it is characterized in that, the content of silicon oxide is 100g/l in the described sodium silicate solution, and the add-on of sodium silicate solution is 5～15% of the covering amount of the silicon oxide titania functional stuffing weight that accounts for preparation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102563542A (en) * | 2009-05-13 | 2012-07-11 | 李欣洋 | LED light source comprising COC (cyclic olefin copolymer) optical filter |
| CN105062149A (en) * | 2015-07-20 | 2015-11-18 | 苏州宇希新材料科技有限公司 | Method for modifying nano-titanium dioxide |
| CN105062204A (en) * | 2015-07-20 | 2015-11-18 | 苏州宇希新材料科技有限公司 | Nano-titanium dioxide printing ink and preparation method thereof |
| CN105131655A (en) * | 2015-07-20 | 2015-12-09 | 苏州宇希新材料科技有限公司 | Nano titanium dioxide modified through liquid silicon deposition |
-
2001
- 2001-04-30 CN CN 01112819 patent/CN1384151A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102563542A (en) * | 2009-05-13 | 2012-07-11 | 李欣洋 | LED light source comprising COC (cyclic olefin copolymer) optical filter |
| CN105062149A (en) * | 2015-07-20 | 2015-11-18 | 苏州宇希新材料科技有限公司 | Method for modifying nano-titanium dioxide |
| CN105062204A (en) * | 2015-07-20 | 2015-11-18 | 苏州宇希新材料科技有限公司 | Nano-titanium dioxide printing ink and preparation method thereof |
| CN105131655A (en) * | 2015-07-20 | 2015-12-09 | 苏州宇希新材料科技有限公司 | Nano titanium dioxide modified through liquid silicon deposition |
| CN105131655B (en) * | 2015-07-20 | 2017-10-24 | 苏州宇希新材料科技有限公司 | The nano titanium oxide that a kind of liquid phase siliceous deposits is modified |
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