CN101062475B - Metasilicate hole material assembled nano titanium oxide composite material and preparation method thereof - Google Patents
Metasilicate hole material assembled nano titanium oxide composite material and preparation method thereof Download PDFInfo
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- CN101062475B CN101062475B CN200610026268.8A CN200610026268A CN101062475B CN 101062475 B CN101062475 B CN 101062475B CN 200610026268 A CN200610026268 A CN 200610026268A CN 101062475 B CN101062475 B CN 101062475B
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Abstract
The invention relates to the making of nanometer titanic anhydride compound material using silicate porous material, with weight percentage of phyllosilicate being 92. 2-95. 9%, and anatase Ti being O27. 8-4. 1%. It is low in processing cost, extended in stone ore application, being able to produce high value-added product with simple process, easy material access, undemanding processing conditions, difficult to pollute, better distribution, effective control of the crystalline dimension, greatly improved in TiO2 compound material feature.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, particularly metasilicate hole material assembled nano titanium oxide composite material and preparation method thereof.
Background technology
Pure TiO
2semi-conductive photoresponse scope is narrower, the recombination probability that semiconductor photoproduction electrons is right is higher, very easily inactivation of excitation state valence band hole and conduction band electron, therefore limited to the degradation effect of organic pollution (as dioxin persistence organic pollutant).TiO
2composite can improve TiO to a certain extent
2activity, but the easily reunion in the preparation of grained catalyst particle is dispersed bad in application, can not fully contact with pollutant.
Early 1990s, in nanometer material science, the compound system of nano particle/mesoporous solid is noticeable.The hole that utilizes the method for physics or chemistry that nano particle is put into micro/meso porous solid forms the assembly system of the two, not only has the numerous characteristics of nanoparticle, and has produced again nanoparticle and the not available special nature of mesoporous solid itself.Meanwhile, be also expected to make people to realize the modulation to some character according to the wish of oneself.This assembly system and metallic/glass composite material, particle mosaic coat, nano composite material etc. are structurally completely different.Because the hole in mesoporous solid is open, and interconnect, therefore, not only there is the interface between heterogeneous nano particle and hole wall in assembly system, and also there is Free Surface in hole endoparticle, and contact with surrounding medium (atmosphere or liquid phase medium), so this assembly system certainly exists the restriction in hole, interface coupling effect, with due to the high activity of nano grain surface to atmosphere around, liquid phase, temperature, the environmental condition sensitivities such as relative humidity (the especially assembly system of metallic particles), thereby make the mesoporous micropore reactor that formed, form the performance of a series of uniquenesses.
Conventionally the method adopting take the nano pore of micro/meso porous material as template assembling function particle has ion-exchange, chemical deposition, absorption object method and hydrothermal synthesis method etc., and assembly object mainly contains simple substance, sulfide, oxide and composite nanometer particle.Katovic has been assembled into metal simple-substance Al, Fe and Zn in pore structure.Found that, the existence of Al, Fe and Zn has changed the acidity of former mesopore molecular sieve, make it likely be applied to acidity, oxidative catalyst field (Microporous andMesoporous Materials, 2001,44～45:275～281), the people such as Li adopt mechanical mixture by SnO
2be assembled in MCM-41 mesopore molecular sieve.Due to the limitation effect of mesopore molecular sieve duct to particle itself, the SnO after assembling
2particle is uniformly distributed in duct, and agglomeration obviously reduces, and the corresponding increase of its specific area impels its selective and sensitiveness to gas all to increase, especially at 250～600 ℃ to H
2susceptibility than pure SnO
2there is significant raising (Sensors and Actuators1999, B 59:1～8).
Also have at present about nanometer Zn FeO
4successfully be assembled into the report in mesoporous silicon matrix, but its heat endurance of prepared product is not ideal.The people such as Zhou are successfully by ZnFeO
4be assembled in silicon mesoporous material, products therefrom not only has expected good magnetic property, and in visible wavelength range, shows the transparency (Materials Chemistry and Physics, 2002,75:181～185).These researchs are to adopt M41S Series Molecules sieve for assembling main body mostly, and the raw material of preparing this molecular sieve analog is mostly organic matter, and cost is higher, and the easy contaminated environment of product.
Hole assembling TiO
2can make TiO
2be evenly distributed in duct, fully contact with pollutant, thereby effectively improve active.In addition because the hole in mesoporous solid is open, and interconnect, therefore, not only there is the interface between heterogeneous nano particle and hole wall in assembly system, and also there is Free Surface in hole endoparticle, and contact with surrounding medium (atmosphere or liquid phase medium), so this assembly system certainly exists the restriction in hole, interface coupling effect, with due to the high activity of nano grain surface to atmosphere around, liquid phase, temperature, the environmental condition sensitivities such as relative humidity (the especially assembly system of metallic particles), thereby make the mesoporous micropore reactor that formed, form the performance of a series of uniquenesses.
But, existing hole assembling TiO
2all to utilize MCM41, must be synthetic by certain chemical technology, more time-consuming.
Summary of the invention
The object of the present invention is to provide metasilicate hole material assembled nano titanium oxide composite material and preparation method thereof, processing cost is low, widens the range of application of Talc Ore simultaneously, produces high value-added product; Technique is simple, and raw material is easy to get, and condition is comparatively loose, is difficult for contaminated environment; Assembled titania is well disperseed, and crystallite dimension is controlled, and the performance of prepared hole assembling TiO2 composite improves a lot before assembling.
Technical scheme of the present invention is, metasilicate hole material assembled nano titanium oxide composite material, and its composition quality percentage is:
Layered phyllosilicate porous material 92.2～95.9
Detitanium-ore-type TiO
27.8～4.1.
The pore volume of phyllosilicate mesoporous material is 0.22ml/g, and pore size distribution range is 1.2～5.5nm, and specific area is 133m
2/ g.The particle size range of the TiO2 assembling is 3.5～6.2nm.
The preparation method of metasilicate hole material assembled nano titanium oxide composite material of the present invention, it comprises the steps:
1) preparation of layered phyllosilicate porous material: taking granularity according to Si/Ti mol ratio in product is the phyllosilicate that is less than 3mm, and Si/Ti mol ratio was got any one value from 10: 1～20: 1, as 10: 1; Pulverize, then with acid solution, under stirring condition, leach, by cooling leachate, filtration, washing, dry, obtain the micro/meso porous material of layered phyllosilicate (material as micro/meso porous in talcum matter);
2) preparation of titanium salt solution: be to measure respectively titanium salt and solvent for 1: 3～1: 8 according to volume ratio, these two kinds of solution are mixed, be fully uniformly dispersed by ultrasonic wave or magnetic agitation, obtain the solution (as the ethanolic solution of butyl titanate) of titanium salt; The object that adds solvent in this operation is for reaction is relaxed;
3) colloidal sol is produced in titanium salt solution and layered phyllosilicate porous material mixing: the beaker that titanium salt solution (as the ethanolic solution of butyl titanate) is housed is placed on magnetic agitation instrument and is stirred, by Si/Ti ratio, be within 10: 1～20: 1, to take above-mentioned steps 1) layered phyllosilicate porous material (material as micro/meso porous in talcum matter) that makes, and this hole material is added in titanium salt solution; After stirring, in molar ratio: water/titanium salt > 1 dropwise adds a certain amount of deionized water, make butyl titanate hydrolysis.In hydrolytic process, by the pH value that acid solution is controlled reaction system, be acid (being pH value < 7), fully, after reaction, stop stirring, obtain colloidal sol;
4) producing of layered phyllosilicate porous material assembled nano titanium oxide composite: utilize above-mentioned steps 3) colloidal sol that obtains, at room temperature ageing, (ageing,, colloidal sol is the colloidal dispersion with fluid characteristics, and the particle of dispersion is solid or large molecule, and gel is the colloidal dispersion with solid features, dispersed material forms continuous mesh skeleton, is filled with liquid or gas in skeleton space.Colloidal sol is slowly polymerization through between ageing micelle, forms the gel of three-dimensional space network structure, has been full of the solvent losing flowability between gel network, forms gel; Gel is prepared the material of molecule and even nanostructured through super-dry, sintering curing.) become gel; With distilled water washing, filter at least twice, then with absolute ethanol washing, filter at least one times, remove remaining organic matter and other impurity; Powder after will washing can make the presoma of layered phyllosilicate porous material assembled nano titanium oxide composite after drying, presoma after grinding at 350～500 ℃ roasting 4～8h obtain layered phyllosilicate porous material assembled nano titanium oxide composite.
Wherein, described titanium salt is butyl titanate, isopropyl titanate, titanium tetrachloride, titanyl sulfate or titanium sulfate; Described phyllosilicate is talcum, kaolinite, pyrophillite, montmorillonite, illite or muscovite;
Described solvent comprises absolute ethyl alcohol, acetylacetone,2,4-pentanedione etc.; Described acid solution is hydrochloric acid, glacial acetic acid.
With planetary mills ball milling 4～6h, ball material weight ratio is 10: 1.
Technology of the present invention is closed and is to seek the catalyst that performance is good, cost is low, environment is had no side effect.This be because dioxin to be a kind of environmental pollution serious and the organic pollution of utmost point difficult degradation, current other common catalyst degradation efficiency are not high or environment is produced to toxicity, and selecting high, the cheap catalyst of a kind of catalytic activity is the pass of realizing dioxin catalytic decomposition in waste gas.
The present invention, on the basis of existing research work, designs the catalyst of different hole material/titanium proportionings, adopts different process schemes, and the finished product that different tests is obtained carries out catalytic test to dioxin.Through adjustment and optimization to hole material/titanium proportioning and technological parameter, and the improvement of catalytic condition nearly 100 times, the hole Material cladding catalyst that can meet dioxin in resolution process waste gas obtained.
Beneficial effect of the present invention
The present invention has the following advantages compared with existing technology:
(1) all to adopt organosilicon and Ludox be raw material to prior art, and through the method preparation assembling main body of hydro-thermal reaction or colloidal sol one glue, raw material are expensive and time-consuming; The present invention prepares micro/meso porous material take phyllosilicate as raw material through chemical treatment, can cut down finished cost, and widens the range of application of Talc Ore simultaneously, produces high value-added product.
(2) technique of the present invention is simple, and raw material is easy to get, and condition is comparatively loose, is difficult for contaminated environment.
(3) because prepared micro/meso porous material contains uniform sequential duct and empty cage is well disperseed assembled titania, crystallite dimension is controlled, and the performance of prepared hole assembling TiO2 composite improves a lot before assembling.
Accompanying drawing explanation
Fig. 1 is the process flow diagram that the present invention prepares stratiform metasilicate hole material assembled nano titanium oxide composite material;
Fig. 2 is the XRD figure of the layered phyllosilicate porous material assembled nano titanium oxide composite before and after assembling;
Fig. 3 is the N of layered phyllosilicate porous material assembled nano titanium oxide composite of the present invention
2adsorption-desorption isothermal curve;
Fig. 4 is the BJH pore size distribution curve of layered phyllosilicate porous material assembled nano titanium oxide composite of the present invention;
Fig. 5 is the HK pore size distribution curve of layered phyllosilicate porous material assembled nano titanium oxide composite of the present invention.
The specific embodiment
Produce the technological process of layered phyllosilicate porous material assembled nano titanium oxide composite as shown in Figure 1:
By planetary mills ball milling 6h for the talcum raw material of-80 orders (0.20mm) granularity (can be also-1mm ,-2mm ,-3mm granularity), ball material weight ratio is 10: 1, after ball milling, with hydrochloric acid, under 80 ℃ of stirring conditions, leach, acid concentration is 4mol/L, extraction time is 2h, by cooling leachate, filtration, washing, dry, obtain the micro/meso porous material of talcum matter (S101).Get 10ml butyl titanate (analyzing pure) and 30ml absolute ethyl alcohol and mix, disperse 10min (S102) with ultrasonic wave.Mixed liquor is used in to heat collecting type constant temperature blender with magnetic force and stirs (S103), according to Si/Ti=10: 1 (mol ratio), in the ethanolic solution of butyl titanate, add talcum matter hole material, in 60 ℃ of water-baths after magnetic agitation 30min, dropwise drip 10ml deionized water, and by HCl or glacial acetic acid solution control pH value in 3.0 left and right, and then stirring 1h (S104), still aging 24h (S105) under room temperature, then the xerogel of ageing is filtered respectively with deionized water and absolute ethyl alcohol in circulating water type vavuum pump, washed twice, after drying at 100 ℃, obtain layered phyllosilicate porous material assembled nano titanium oxide composite material precursor (S106) in electric heating constant-temperature blowing drying box.With box-shaped resistance furnace roasting 4h (S107) at 350 ℃, 400 ℃, 500 ℃ respectively, can obtain Si/Ti mol ratio and be the layered phyllosilicate porous material assembled nano titanium oxide composite (S108) of 10: 1.
The XRD that makes product schemes as shown in Figure 2, and Fig. 2 is the XRD figure of the layered phyllosilicate porous material assembled nano titanium oxide composite that at presoma and 350 ℃, roasting obtains.(a-talcum matter hole material; B-hole assembling TiO
2composite).
As seen from the figure,, there is Detitanium-ore-type TiO in roasting at 350 ℃
2, also have some amorphous substances.The component content of the layered phyllosilicate porous material assembled nano titanium oxide composite making is as shown in table 1 below.
The content (%) of each phase in the material assembled nano titanium oxide composite of the different embodiment of table 1 hole
N
2adsorption-desorption isothermal curve, as shown in Figure 3, can find out successfully prepared TiO
2the specific area of/hole material powder is by the 260.20m before assembling
2/ g drops to 189.50m
2/ g, pore volume drops to 0.40ml/g by 0.51ml/g, and after assembling, micropore quantity reduces, and this absolutely proves TiO
2successfully be assembled into micro-mesoporous in.
BJH pore size distribution curve, as shown in Figure 4, as shown in Figure 5, pore size distribution range is 1.2～5.5nm to HK pore size distribution curve.
TiO
2it itself is a kind of semiconductor nano catalyst, after being assembled into layered phyllosilicate porous material, will greatly improve its catalytic activity, can be used as the efficient decomposition catalyst of dioxin persistence organic pollutant, be applied to the reduction of discharging process field of dioxin in the waste gas of steel industry, waste incineration industry etc.The advantages such as Yttria/titanium dioxide nano composite material oxidability prepared by the present invention is strong, and catalytic activity is high, nontoxic, biological, chemical, photochemical stability is good, can be used for the fields such as sewage disposal, air cleaning, sterilization, energy and material.
The present invention can be applied to the reduction of discharging of the dioxin persistence organic pollutant in sintering and electric furnace production discharging waste gas and process above, and can be applied to the exhaust-gas treatment of domestic iron and steel enterprise, waste incineration industry.In steel industry worldwide and incineration treatment of garbage industry, there are wide promotional value and application prospect.
Claims (7)
1. metasilicate hole material assembled nano titanium oxide composite material, its composition quality percentage is:
Layered phyllosilicate porous material 92.2～95.9
Detitanium-ore-type TiO
27.8～4.1;
The pore volume of described composite is 0.22～0.40ml/g, and pore size distribution range is 1.2～5.5nm, and specific area is 133～189m
2/ g;
Described composite is that the method by comprising following steps is manufactured:
1) preparation of layered phyllosilicate porous material: take granularity according to Si/Ti mol ratio in product small in the phyllosilicate of 3mm, Si/Ti mol ratio is got any one value from 10: 1～20: 1, pulverize, then with acid solution, under stirring condition, leach, by cooling leachate, filtration, washing, dry, obtain the micro/meso porous material of layered phyllosilicate;
2) preparation of metatitanic acid solution: be to measure respectively titanium salt and solvent for 1: 3～1: 8 according to volume ratio, the two is mixed, be fully uniformly dispersed by ultrasonic wave or magnetic agitation, obtain titanium salt solution;
3) colloidal sol is produced in titanium salt solution and layered phyllosilicate porous material mixing: the beaker that titanium salt solution is housed is placed in to stir on instrument and stirs, by Si/Ti mol ratio, be within 10: 1～20: 1, to take above-mentioned steps 1) layered phyllosilicate porous material that makes, and this hole material is added in titanium salt solution; After stirring, in molar ratio: water/titanium salt > 1 dropwise adds deionized water, described titanium salt being decomposed, is acidity by the pH value that acid solution is controlled reaction system in hydrolytic process; Fully, after reaction, stop stirring, obtain colloidal sol;
4) further produce layered phyllosilicate porous material assembled nano titanium oxide composite: utilize above-mentioned steps 3) colloidal sol that obtains, at room temperature ageing, becomes gel; With distilled water washing, filter at least twice, then with absolute ethanol washing, filter at least one times, remove remaining organic matter and other impurity; After being dried, powder after washing can make the precursor of phyllosilicate ester hole material assembled nano titanium oxide composite material; Precursor after grinding again at 350-500 ℃ roasting 4-8h obtain layered phyllosilicate porous material assembled nano titanium oxide composite.
2. metasilicate hole material assembled nano titanium oxide composite material as claimed in claim 1, is characterized in that, layered phyllosilicate porous material comprises talcum, kaolinite, pyrophillite, montmorillonite, illite or dolomite.
3. metasilicate hole material assembled nano titanium oxide composite material as claimed in claim 1, is characterized in that, TiO
2particle size range be 3.5～6.2nm.
4. the preparation method of metasilicate hole material assembled nano titanium oxide composite material as claimed in claim 1, is characterized in that, described titanium salt is butyl titanate, isopropyl titanate, titanium tetrachloride, titanyl sulfate or titanium sulfate.
5. the preparation method of metasilicate hole material assembled nano titanium oxide composite material as claimed in claim 1, is characterized in that, described acid solution is hydrochloric acid or glacial acetic acid.
6. the preparation method of metasilicate hole material assembled nano titanium oxide composite material as claimed in claim 1, is characterized in that, described solvent is absolute ethyl alcohol or acetylacetone,2,4-pentanedione.
7. the preparation method of metasilicate hole material assembled nano titanium oxide composite material as claimed in claim 1, is characterized in that step 1) and 3) stirring adopt ultrasonic wave or magnetic agitation instrument to stir.
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| CN102500313B (en) * | 2011-10-13 | 2013-09-04 | 湖南文象炭基环保材料股份有限公司 | Preparation method of nano semiconductor material loaded on silicate substrate |
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| CN110038616A (en) * | 2019-04-23 | 2019-07-23 | 襄阳先创环保科技有限公司 | A kind of municipal sewage treatment agent |
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| CN116618050B (en) * | 2023-04-20 | 2024-01-12 | 陕西科技大学 | Titanium dioxide/ferric silicate heterojunction photo-Fenton catalyst, preparation method and application |
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