CN100998933A - Organic clay loaded with nanometer anatase type titanium dioxide and its preparation method and use - Google Patents
Organic clay loaded with nanometer anatase type titanium dioxide and its preparation method and use Download PDFInfo
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Abstract
A organic clay carrying nano-class anatase-type TiO2 is prepared from clay through modifying it by long-chain alkyl ammonium salt and carrying the anatase-type TiO2 nanoparticles by sol-gel method. It can be used as a photocatalyst for photodecomposing the organic pollutant in sewage or photodegradating polymer.
Description
Technical field
The present invention relates to organic clay of a kind of loaded with nanometer anatase type titanium dioxide and preparation method thereof, and this organic clay is used for decomposition of water organic pollution light and the photodegradative purposes of polymer.
Background technology
Titanium dioxide has the stable and eco-friendly characteristics of photocatalytic activity height, chemical property as photochemical catalyst and is widely used.Titanium dioxide has three kinds of crystal formations usually: anatase, rutile and brockite.Wherein, Detitanium-ore-type is because the ability of stronger adsorb oxygen and the band gap (3.2eV) of broad, can absorbing wavelength less than the ultraviolet light of 380nm, have excellent photocatalysis activity.
The photocatalytic activity of titanium dioxide and crystallite dimension size are closely related, and particle size determines photic electrons/to efficient compound and that shift to substrate again.When the titanium dioxide particle diameter reduced, photic electronics and cavity energy were moved to the surface rapidly, reduced this right bluk recombination of electrons/, improved quantum yield, can greatly improve photocatalytic activity.Chinese patent CN01125659.1 discloses a kind of preparation method of Nanotitanium dioxide column supported bentonite, is the pillared thing of the titanium dioxide below the particle diameter 1nm is embedded in passage between bentonite bed.But reducing of photocatalytic activity raising and particle diameter is not linear dependence, and when particle diameter was reduced to a certain degree, electrons/increased the probability of surface recombination, and photocatalytic activity is reduced.Discover that when particle diameter during in the 10nm left and right sides, titanium dioxide has the strongest absorption luminous energy power and the highest photocatalytic activity [J.Phys.Chem.B 10871 (1998)].
In actual application, superfine nano titanium dioxide is very easily reunited, and forms bigger particle, influences its photocatalysis efficiency.Therefore, in the application process of nano titanium oxide, must consider its dispersiveness.Titanium dichloride load on matrix, as [US Patent No.5981426] on aluminium oxide and the silica, can be obtained the nano-titania particle of high dispersive, and has bigger specific area and smaller particle size.Chinese patent CN1265939A discloses a kind of preparation method of load type titania photocatalyst, and this method is to be carrier with the concavo-convex rod of natural minerals clay, and nano titanium oxide suspension slurry and carrier mixed calcining are made.This method can not play real peptizaiton to titanium dioxide, also can cause the sintering of titanium dioxide in high-temperature calcination process, makes particle diameter increase surface area and reduces.
Summary of the invention
First purpose of the present invention provide load particle diameter be the organic clay of 2～50nm anatase-type nanometer titanium dioxide.
Second purpose of the present invention provides a kind of preparation method of organic clay of loaded with nanometer anatase type titanium dioxide.
The organic clay that the 3rd purpose of the present invention provides loaded with nanometer anatase type titanium dioxide be used for that water organic pollution light decomposes and the polymer light degradation aspect purposes.
The organic clay of loaded with nanometer anatase type titanium dioxide of the present invention has the advantage that specific area is big, adsorptivity is strong, photocatalytic activity is high, especially its hydrophobic property, help contacting with organic pollution in the water, improve photocatalysis efficiency, be convenient to the recovery of catalyst, also help and realize that in polymer homogeneous disperses, as the polymer Photodegradation catalyst.
In the organic clay of loaded with nanometer anatase type titanium dioxide of the present invention, the load factor of nano-anatase mine-titanium oxide is 75～95%, and nano-anatase mine-titanium oxide accounts for 5～80% of gross mass.Described nano-anatase mine-titanium oxide distribution of particles is middle and sheet surfaces in the lamella of organic clay.
The particle diameter of nano-anatase mine-titanium oxide of the present invention is 2～50nm, and particle size is controlled.
The organic clay of loaded with nanometer anatase type titanium dioxide of the present invention, at first clay is organised by cation exchange, adsorbing organically-modified technology, utilize sol-gel processing again, with the hydrolysis of titanium precursor body and be condensed into nano-anatase mine-titanium oxide, then the nano-anatase mine-titanium oxide that generates is loaded on the organic clay, make the organic clay of loaded with nanometer anatase type titanium dioxide.
The preparation method of the organic clay of loaded with nanometer anatase type titanium dioxide of the present invention may further comprise the steps:
(1) clay is distributed to the suspension that forms 0.5～10wt% in the water, adds molal quantity and be 0.5～2 times of chain alkyl ammonium salt to the clay cation exchange capacity in 70～85 ℃ of dissolvings;
(2) the titanium precursor body is dissolved into forms solution in the alcohol, join that reaction is to forming clear solution in the acid solution, wherein, titanium precursor body: alcohol: the mol ratio of acid is 1: 5～25: 4～10;
(3) clear solution with step (2) slowly joins in the clay suspension of step (1), 40～100 ℃ of stirrings, and wherein, the consumption of titanium is 1～60mmol/g clay;
(4) product that step (3) is obtained separates, and isolates solid and dry, and dried product is pulverized, and obtains the organic clay of loaded with nanometer anatase type titanium dioxide.
Clay of the present invention has adsorptivity, expansiveness, cation exchange and higher dispersed and bigger surface area, is selected from one or more the mixture in montmorillonite, hectorite, saponite, rectorite, nontronite, the vermiculite.
It is 12～18 chain alkyl that chain alkyl ammonium salt of the present invention contains one or two carbon numbers, is selected from DTAC, DTAB, tetradecyl trimethyl ammonium chloride, TTAB, hexadecyltrimethylammonium chloride, softex kw, OTAC, the octadecyl trimethylammonium bromide, dodecyl benzyl dimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, the myristyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium, cetalkonium chloride, cetyl dimethyl benzyl ammonium bromide, stearyl dimethyl benzyl ammonium chloride, octadecyl dimethyl benzyl ammonium bromide, Varisoft 432PPG, double hexadecyl dimethyl ammonium bromide, dioctadecyl dimethyl ammonium chloride, the mixture of one or more in two octadecyl dimethyl ammonium bromides.The molal quantity of chain alkyl ammonium salt is 0.5～2 times of cation exchange capacity to clay, and purpose is the hydrophobicity of regulating organic clay.
Titanium precursor body of the present invention is selected from a kind of in tetra-n-butyl titanate, metatitanic acid four isobutyl esters, tetraisopropyl titanate, metatitanic acid four n-propyls, tetraethyl titanate, metatitanic acid butyl isopropyl esters, metatitanic acid four monooctyl esters, metatitanic acid mixed ester, the titanium tetrachloride.
Alcohol of the present invention is selected from a kind of in ethanol, isopropyl alcohol, n-butanol, the methyl alcohol.
Acid of the present invention can be inorganic acid, is selected from a kind of in hydrochloric acid, nitric acid, sulfuric acid, the phosphoric acid; Can be organic acid also, be selected from a kind of in acetic acid, acrylic acid, the citric acid; It also can be the mixture of above-mentioned acid.
The organic clay of loaded with nanometer anatase type titanium dioxide of the present invention decomposes and the photodegradative photocatalyst applications of polymer as organic pollution light in the water.
The advantage of the organic clay of loaded with nanometer anatase type titanium dioxide of the present invention is:
1) nano-titania particle is distributed on organic clay sheet interlayer and the lamella, has stoped the reunion of nano titanium oxide in application process, and can effectively control the particle diameter of nano-anatase mine-titanium oxide by changing experiment condition;
2) distinctive hydrophobic property behind the clay organic modification helps organic pollution and homogeneous dispersion in polymer in the adsorbed water;
3) nano-anatase mine-titanium oxide has higher photocatalytic activity under lower content;
When 4) being used for the light decomposition of sewage disposal organic pollution, be convenient to the recovery of catalyst;
5) cheap as the clay of primary raw material, can reduce product cost.
Description of drawings
Fig. 1. the X-ray diffractogram of the organic montmorillonite of raw material montmorillonite, organically modified montmorillonite clay and the loaded with nanometer anatase type titanium dioxide of the embodiment of the invention 1.
(A): the raw material montmorillonite; (B): organically modified montmorillonite clay; (C): the organic montmorillonite of loaded with nanometer anatase type titanium dioxide.
Fig. 2. the Raman spectrum of the organic montmorillonite of raw material montmorillonite, organically modified montmorillonite clay and the loaded with nanometer anatase type titanium dioxide of the embodiment of the invention 2.
(A): the raw material montmorillonite; (B): organically modified montmorillonite clay; (C): the organic montmorillonite of loaded with nanometer anatase type titanium dioxide.
Fig. 3. the transmission electron microscope photo of the organic clay of the loaded with nanometer anatase type titanium dioxide of the embodiment of the invention 3: (A) low resolution transmission electron microscope photo; (B) high-resolution transmission electron microscope photo.
The specific embodiment
Below in conjunction with embodiment technical characterictic of the present invention is described, need to prove that these just part descriptions for example do not constitute the restriction to content of the present invention.
Embodiment 1
Clay organically-modified: the 5g montmorillonite is dispersed in the 500ml deionized water and forms steady suspension.Take by weighing the 1.64g softex kw and join 80 ℃ of stirring and dissolving in the montmorillonite suspension.
The hydrolysis under acid condition of titanium precursor body alcoholic solution: the 17ml tetra-n-butyl titanate is dissolved in the ethanol of 34ml, and slowly joining the 250ml molar concentration is in the HCl solution of 1mol/L, and 25 ℃ of vigorous stirring are to forming clear solution.
The load of nano titanium oxide on organic clay: prepared clear solution dropwise is added drop-wise in the suspension of montmorillonite, 80 ℃ are stirred 10h.Suction filtration, and the pH that is washed with water to filtrate is 6～7.Isolate solid, 100 ℃ of vacuum drying, grind into powder obtains the nano-anatase mine-titanium oxide distribution of particles in the middle of the lamella of organic clay and the organic montmorillonite of the loaded with nanometer anatase type titanium dioxide of sheet surfaces.
Embodiment 2
Clay organically-modified: the 5g montmorillonite is dispersed in the 500ml deionized water and forms steady suspension.Take by weighing the 2.64g dioctadecyl dimethyl ammonium chloride and join 80 ℃ of stirring and dissolving in the montmorillonite suspension.
The hydrolysis under acid condition of titanium precursor body alcoholic solution: the 17ml tetra-n-butyl titanate is dissolved in the ethanol of 34ml, slowly joins the H that the 250ml molar concentration is 1mol/L
3PO
4In the solution, 25 ℃ of vigorous stirring are to forming clear solution.
The load of nano titanium oxide on organic clay: prepared clear solution dropwise is added drop-wise in the suspension of montmorillonite, 80 ℃ are stirred 10h.Suction filtration, and the pH that is washed with water to filtrate is 6～7.Isolate solid, 100 ℃ of vacuum drying, grind into powder obtains the nano-anatase mine-titanium oxide distribution of particles in the middle of the lamella of organic clay and the organic montmorillonite of the loaded with nanometer anatase type titanium dioxide of sheet surfaces.
Embodiment 3
Clay organically-modified: the 5g vermiculite is dispersed in the 500ml deionized water and forms steady suspension.Take by weighing the 1.70g hexadecyltrimethylammonium chloride and join 80 ℃ of stirring and dissolving in the vermiculite suspension.
The hydrolysis under acid condition of titanium precursor body alcoholic solution: the 14.2ml tetraisopropyl titanate is dissolved in the ethanol of 28.4ml, and slowly joining the 250ml molar concentration is in the HCl solution of 1mol/L, and 25 ℃ of vigorous stirring are to forming clear solution.
The load of nano titanium oxide on organic clay: prepared clear solution dropwise is added drop-wise in the suspension of vermiculite, 80 ℃ are stirred 10h.Suction filtration, and the pH that is washed with water to filtrate is 6～7.Isolate solid, 100 ℃ of vacuum drying, grind into powder obtains the nano-anatase mine-titanium oxide distribution of particles in the middle of the lamella of organic clay and organic vermiculite of the loaded with nanometer anatase type titanium dioxide of sheet surfaces.
Embodiment 4
Clay organically-modified: the 5g hectorite is dispersed in the 500ml deionized water and forms steady suspension.Take by weighing 4.8g octadecyl dimethyl benzyl ammonium bromide and join 80 ℃ of stirring and dissolving in the hectorite suspension.
The hydrolysis under acid condition of titanium precursor body alcoholic solution: the 17ml tetra-n-butyl titanate is dissolved in the ethanol of 34ml, and slowly joining the 250ml molar concentration is in the HCl solution of 1mol/L, and 25 ℃ of vigorous stirring are to forming clear solution.
The load of nano titanium oxide on organic clay: prepared clear solution dropwise is added drop-wise in the suspension of hectorite 80 ℃ of stirrings.Suction filtration, and the pH that is washed with water to filtrate is 6～7.Isolate solid, 100 ℃ of vacuum drying, grind into powder obtains the nano-anatase mine-titanium oxide distribution of particles in the middle of the lamella of organic clay and the organolithium montmorillonite of the loaded with nanometer anatase type titanium dioxide of sheet surfaces.
Embodiment 5
Clay organically-modified: the 10g montmorillonite is dispersed in the 500ml deionized water and forms steady suspension.Take by weighing the 4g cetyl dimethyl benzyl ammonium bromide and join 80 ℃ of stirring and dissolving in the montmorillonite suspension.
The hydrolysis under acid condition of titanium precursor body alcoholic solution: the 19ml titanium tetrachloride is dissolved in the 20ml ethanol, and slowly joining the 160ml molar concentration is in the HCl solution of 3mol/L, and vigorous stirring forms clear solution.
The load of nano titanium oxide on organic clay: prepared clear solution dropwise is added drop-wise in the suspension of montmorillonite 80 ℃ of stirrings.Suction filtration, and the pH that is washed with water to filtrate is 6～7.Isolate solid, 100 ℃ of vacuum drying, grind into powder obtains the nano-anatase mine-titanium oxide distribution of particles in the middle of the lamella of organic clay and the organic montmorillonite of the loaded with nanometer anatase type titanium dioxide of sheet surfaces.
Embodiment 6
Clay organically-modified: the 5g nontronite is dispersed in the 500ml deionized water and forms steady suspension.Take by weighing the 1.5g cetyl dimethyl benzyl ammonium bromide and join 80 ℃ of stirring and dissolving in the nontronite suspension.
The hydrolysis under acid condition of titanium precursor body alcoholic solution: the 17ml tetra-n-butyl titanate is dissolved in the ethanol of 34ml, slowly joins the HNO that the 250ml molar concentration is 1mol/L
3In the solution, 25 ℃ of vigorous stirring are to forming clear solution.
The load of nano titanium oxide on organic clay: prepared clear solution dropwise is added drop-wise in the suspension of nontronite, 80 ℃ are stirred 10h.Suction filtration, and the pH that is washed with water to filtrate is 6～7.Isolate solid, 100 ℃ of vacuum drying, grind into powder obtains the nano-anatase mine-titanium oxide distribution of particles in the middle of the lamella of organic clay and organic nontronite of the loaded with nanometer anatase type titanium dioxide of sheet surfaces.
Embodiment 7
Clay organically-modified: 2.5g montmorillonite and 2.5g rectorite are dispersed in the 500ml deionized water and form steady suspension.Take by weighing 1.7g octadecyl trimethylammonium bromide and join 80 ℃ of stirring and dissolving in the suspension.
The hydrolysis under acid condition of titanium precursor body alcoholic solution: the 14.2ml tetraisopropyl titanate is dissolved in the isopropyl alcohol of 28.4ml, and slowly joining the 250ml molar concentration is in the HCl solution of 1mol/L, and 25 ℃ of vigorous stirring are to forming clear solution.
The load of nano titanium oxide on organic clay: prepared clear solution dropwise is added drop-wise in the mixing suspension of montmorillonite and rectorite 80 ℃ of stirrings.Suction filtration, and the pH that is washed with water to filtrate is 6～7.Isolate solid, 100 ℃ of vacuum drying, grind into powder obtains the nano-anatase mine-titanium oxide distribution of particles in the middle of the lamella of organic clay and the organic clay of the loaded with nanometer anatase type titanium dioxide of sheet surfaces.
Embodiment 8
Clay organically-modified: the 10g montmorillonite is dispersed in the 500ml deionized water and forms steady suspension.Take by weighing the 3.5g OTAC and join 80 ℃ of stirring and dissolving in the montmorillonite suspension.
The hydrolysis under acid condition of titanium precursor body alcoholic solution: the 17ml tetra-n-butyl titanate is dissolved in the isopropyl alcohol of 34ml, and slowly joining the 250ml molar concentration is in the HCl solution of 1mol/L, and 25 ℃ of vigorous stirring are to forming clear solution.
The load of nano titanium oxide on organic clay: prepared clear solution dropwise is added drop-wise in the suspension of montmorillonite, 80 ℃ are stirred 10h.Suction filtration, and the pH that is washed with water to filtrate is 6～7.Isolate solid, 100 ℃ of vacuum drying, grind into powder obtains the nano-anatase mine-titanium oxide distribution of particles in the middle of the lamella of organic clay and the organic montmorillonite of the loaded with nanometer anatase type titanium dioxide of sheet surfaces.
Embodiment 9
Clay organically-modified: the 2.5g montmorillonite is dispersed in the 500ml deionized water and forms steady suspension.Take by weighing the 0.82g softex kw and join 80 ℃ of stirring and dissolving in the montmorillonite suspension.
The hydrolysis under acid condition of titanium precursor body alcoholic solution: the 17ml tetra-n-butyl titanate is dissolved in the ethanol of 34ml, slowly joins the H that the 250ml molar concentration is 1mol/L
2SO
4In the solution, 25 ℃ of vigorous stirring are to forming clear solution.
The load of nano titanium oxide on organic clay: prepared clear solution dropwise is added drop-wise in the suspension of montmorillonite, 80 ℃ are stirred 10h.Suction filtration, and the pH that is washed with water to filtrate is 6～7.Isolate solid, 100 ℃ of vacuum drying, grind into powder obtains the nano-anatase mine-titanium oxide distribution of particles in the middle of the lamella of organic clay and the organic montmorillonite of the loaded with nanometer anatase type titanium dioxide of sheet surfaces.
Clay organically-modified: the 5g rectorite is dispersed in the 500ml deionized water and forms steady suspension.Take by weighing the 1.64g softex kw and join 80 ℃ of stirring and dissolving in the rectorite suspension.
The hydrolysis under acid condition of titanium precursor body alcoholic solution: the 17ml tetra-n-butyl titanate is dissolved in the ethanol of 34ml, slowly joins the 250ml mass fraction then and is in 80% the acetum, and 25 ℃ of vigorous stirring 3h form pale yellow solution.
The load of nano titanium oxide on organic clay: prepared pale yellow solution dropwise is added drop-wise in the suspension of rectorite, 80 ℃ are stirred 10h.Suction filtration, and the pH that is washed with water to filtrate is 6～7.Isolate solid, 100 ℃ of vacuum drying, grind into powder obtains the nano-anatase mine-titanium oxide distribution of particles in the middle of the lamella of organic clay and the organic rectorite of the loaded with nanometer anatase type titanium dioxide of sheet surfaces.
Claims (10)
1. the organic clay of a loaded with nanometer anatase type titanium dioxide, it is characterized in that: the load factor of nano-anatase mine-titanium oxide is 75～95% in this organic clay, and nano-anatase mine-titanium oxide accounts for 5～80% of gross mass.
2. the organic clay of loaded with nanometer anatase type titanium dioxide according to claim 1 is characterized in that: described nano-anatase mine-titanium oxide distribution of particles is in the middle of the lamella of organic clay and sheet surfaces.
3. the organic clay of loaded with nanometer anatase type titanium dioxide according to claim 1 and 2, it is characterized in that: the particle diameter of described nano-anatase mine-titanium oxide is 2～50nm.
4. the organic clay of loaded with nanometer anatase type titanium dioxide according to claim 1 and 2 is characterized in that: described clay is selected from one or more the mixture in montmorillonite, hectorite, saponite, rectorite, nontronite, the vermiculite.
5. the preparation method according to the organic clay of each described loaded with nanometer anatase type titanium dioxide of claim 1～4 is characterized in that, this method may further comprise the steps:
(1) clay is distributed to the suspension that forms 0.5～10wt% in the water, adds molal quantity and be 0.5～2 times of chain alkyl ammonium salt to the clay cation exchange capacity in 70～85 ℃ of dissolvings;
(2) the titanium precursor body is dissolved into forms solution in the alcohol, join that reaction is to forming clear solution in the acid solution, wherein, titanium precursor body: alcohol: the mol ratio of acid is 1: 5～25: 4～10;
(3) clear solution with step (2) slowly joins in the clay suspension of step (1), 70～85 ℃ of stirrings, and wherein, the consumption of titanium is 1～60mmol/g clay;
(4) product that step (3) is obtained separates, and isolates solid and dry, and dried product is pulverized, and obtains the organic clay of loaded with nanometer anatase type titanium dioxide.
6. method according to claim 5, it is characterized in that: it is 12～18 chain alkyl that described chain alkyl ammonium salt contains one or two carbon numbers, is selected from DTAC, DTAB, tetradecyl trimethyl ammonium chloride, TTAB, hexadecyltrimethylammonium chloride, softex kw, OTAC, the octadecyl trimethylammonium bromide, dodecyl benzyl dimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, the myristyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium, cetalkonium chloride, cetyl dimethyl benzyl ammonium bromide, stearyl dimethyl benzyl ammonium chloride, octadecyl dimethyl benzyl ammonium bromide, Varisoft 432PPG, double hexadecyl dimethyl ammonium bromide, dioctadecyl dimethyl ammonium chloride, the mixture of one or more in two octadecyl dimethyl ammonium bromides.
7. method according to claim 5 is characterized in that: described titanium precursor body is selected from a kind of in tetra-n-butyl titanate, tetraisopropyl titanate, tetraethyl titanate, metatitanic acid four isobutyl esters, metatitanic acid four n-propyls, metatitanic acid butyl isopropyl esters, metatitanic acid four monooctyl esters, metatitanic acid mixed ester, the titanium tetrachloride.
8. method according to claim 5 is characterized in that: described alcohol is selected from a kind of in ethanol, isopropyl alcohol, n-butanol, the methyl alcohol.
9. method according to claim 5 is characterized in that: described acid is selected from hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, acetic acid, acrylic acid, the citric acid one or more mixture.
10. purposes according to the organic clay of each described loaded with nanometer anatase type titanium dioxide of claim 1～4 is characterized in that: this organic clay decomposes and the photodegradative photocatalyst applications of polymer as organic pollution light in the water.
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