CN103551136B - Attapulgite loaded quasi-one-dimensional titanium dioxide composite photocatalyst and preparation method thereof - Google Patents
Attapulgite loaded quasi-one-dimensional titanium dioxide composite photocatalyst and preparation method thereof Download PDFInfo
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- CN103551136B CN103551136B CN201310449740.9A CN201310449740A CN103551136B CN 103551136 B CN103551136 B CN 103551136B CN 201310449740 A CN201310449740 A CN 201310449740A CN 103551136 B CN103551136 B CN 103551136B
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Abstract
The invention relates to the technical fields of nano-materials and photocatalysis, in particular to an attapulgite loaded quasi-one-dimensional titanium dioxide composite photocatalyst and a preparation method thereof. The carrier of the composite photocatalyst is attapulgite, and pine needle shaped nano-scale titanium dioxide particles are uniformly distributed on the surface of the attapulgite. The preparation method includes hydrolytic precipitation loading of nano-titanium dioxide and subsequent heat treatment processes. The composite photocatalyst provided by the invention is prepared by a hydrolytic precipitation loading technique. Attapulgite is taken as the carrier to make the quasi-one-dimensional nano-TiO2 particles fixed on the surface to form a stable TiO2/attapulgite photocatalyst. The quasi-one-dimensional pine needle shaped nano-scale iO2 particles are uniformly distributed on the surface of the attapulgite, so that agglomeration of TiO2 particles can be avoided, and the problems of TiO2 photocatalyst specific surface area decrease and photocatalytic performance degradation caused by the agglomeration effect cannot appear. At the same time, without additional equipment and energy consumption, recovery and reuse of the photocatalyst can be realized.
Description
Technical field
The present invention relates to nano material and photocatalysis technology field, specifically accurate one-dimensional titanium dioxide composite photo-catalyst of a kind of attapulgite load and preparation method thereof.
Background technology
The application of photocatalysis technology in degradation of contaminant oneself become one of focus of countries nowadays field of environment protection research.In numerous semiconductor light-catalyst, nano titanium oxide TiO
2receive much attention because of outstanding advantages such as it is nontoxic, cheap, stable chemical nature, catalytic efficiency are high, non-secondary pollution, applied ranges.Nano-TiO
2the use of photochemical catalyst mainly contains two kinds of forms, namely directly uses nano-TiO
2particle suspend carry out in the solution catalytic reaction suspension system and by nano-TiO
2the load system of catalytic reaction is carried out in load on carrier substrate.Photocatalysis Problems existing based on suspension system is by TiO
2separate from water and need extra device and be difficult to be separated cost-effectively, there is the difficulty such as the practical application that is difficult to dispersion, recovery.Simultaneously in running due to small-size effect, nano-TiO
2in dispersion, easily reunion, sedimentation leakage cause light utilization efficiency low in existence.In addition, the general concentration of organic pollution is low, at TiO
2the adsorptivity of photocatalyst surface is poor, there is photocatalytic degradation speed slow, need the long period just can reach degradable shortcoming in practical application.These problems limit suspended nano TiO
2the application and development of photochemical catalyst.
Adopt that specific area is large in recent years, the Inert absorbent of porous is as carrier and nano-TiO
2compound Kaolinite Preparation of Catalyst has become TiO
2an important development trend and direction in photocatalysis research field.Conventional and nano-TiO
2composite adsorption active carrier material comprises synthesis of molecular sieve, active carbon, zeolite, sepiolite, various synthesis of nano Porous materials etc.
Attapulgite is also known as palygorskite, be a kind of have layer chain crystal structure containing Shuifu County's zeopan natural nano-mineral material, its transmission electron microscope photo can consult Fig. 1, it has low-dimensional, (crystal diameter is generally 40 ~ 50nm to nanoscale, length hundreds of nanometer to several microns, has very large Extra specific surface area sum inner ratio surface area), containing nanoscale pore passage structure, containing the design features such as the crystallization water and excellent absorption, ion-exchange, corrosion-resistant, resistance to oxidation, high-temperature physics stable chemical performance and lightweight (2.0 ~ 3.0g/cm
3) etc. performance, also have wide material sources, cheap advantage (for Mingguang City, Anhui Province richness produce attapulgite, the powder market price of 2008 after purified is about 1000 yuan per ton), be a kind of catalyst carrier material of great potential.
The patent No. is the patent of invention of ZL2010102704468, discloses a kind of PS-TiO
2the preparation method of-ATP organic/inorganic composite film first PS is dissolved in C
6h
12in obtain solution A, secondly nano-TiO
2/ ATP composite granule is dispersed in C
6h
12in obtain B solution, then solution A and B solution are carried out ultrasonicly being mixed to get C solution, finally on the thin slice cleaned, pour C solution into, spin-coating film, naturally dry, through 100 ~ 110 DEG C of heat treatments, obtain PS-TiO
2-ATP organic/inorganic composite film.This film can be applicable to the occasions such as photocatalysis, solar film battery, opto-electronic conversion, thermoelectricity conversion, electromagnetic shielding, microwave absorption.
The patent No. is the patent of invention of ZL2008100208841, discloses a kind of preparation method of nanometer titanium dioxide/attapulgite composite material, is first to be joined in deionized water by attapulgite to be mixed with slurry; In nano-TiO 2 precursor, add attapulgite slurry again, form the molecular blue and white glue of nano titanium oxide/attapulgite clay compounded grain; Finally with alkaline solution by glue adjust ph, refilter cyclic washing to remove the foreign ion in filter cake; By the filtration cakes torrefaction of gained, be prepared into nano titanium oxide/concave convex rod composite material powder.
Summary of the invention
For the technical problem existed in prior art, the present invention is intended to solve that conventional suspension system nano titanium dioxide photocatalyst is easily reunited, difficult dispersion, photocatalysis efficiency are low, and light degradation terminates the technological deficiency of rear separation and recovery difficulty, provide accurate one-dimensional titanium dioxide composite photo-catalyst of a kind of attapulgite load and preparation method thereof, the nanoscale TiO of accurate one dimension pine needle shape pattern can be made
2be evenly dispersed in attapulgite on the surface, avoid TiO
2the reunion of particle, therefore there will not be because of the TiO caused by reuniting effect
2the problem that the reduction of photochemical catalyst specific area and photocatalysis performance decline.
To achieve these goals, the technical solution adopted in the present invention is: the accurate one-dimensional titanium dioxide composite photo-catalyst of a kind of attapulgite load, the carrier of this composite photo-catalyst is attapulgite, and the surface uniform of described attapulgite is distributed with the Nano titanium dioxide particle in pine needle pattern.
The preparation method of the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load, comprise hydrolytic precipitation load and the follow-up heat treatment process of nano titanium oxide, concrete steps are as follows:
1. 10 ~ 50g/L attapulgite deionized water suspension I, is prepared;
2., under the magnetic agitation condition of ice-water bath and 150 ~ 400r/min, be the TiCl of 98% by 2.5 ~ 7.0ml concentration
4it is in the sulfuric acid solution of 5 ~ 30% that solution drops to 10 ~ 30ml concentration, then adds the TiCl that deionized water compound concentration is 0.05 ~ 0.5mol/L
4the aqueous solution;
3., get 50 ~ 150mL suspension I and put into beaker, regulate suspension pH value to 2.0 ~ 3.5 with dilute sulfuric acid, beaker is placed in the water bath with thermostatic control of 80 ~ 90 DEG C, maintain the mechanical agitation of 150 ~ 400r/min, and add 15 ~ 25g sustained release agent, obtain suspension II;
4., with by TiCl
4the aqueous solution drops in suspension II, drips off rear continuation stirring 20 ~ 40min;
5., centrifugal recovery sediment, to wash to pH in neutral, collecting precipitation thing, obtains the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load through super-dry, roasting successively.
Preferably, step 3. in sustained release agent be urea.
Preferably, step 4. in rate of addition be 1mL/min.
Preferably, step 5. in washing be adopt the alternately washing of distilled water and absolute ethyl alcohol.
Preferably, step 5. middle baking temperature is 60 ~ 80 DEG C, and sintering temperature is 400 ~ 500 DEG C, and roasting time is 1 ~ 2h.
Further, preparation steps 1. described attapulgite deionized water suspension I time be also provided with attapulgite pre-treatment step, this pre-treatment step is specially: first prepare 10 ~ 50g/L attapulgite deionized water suspension, then add concentrated hydrochloric acid and obtain mixed solution, carry out successively activating, leave standstill, centrifugal, wash to pH value to be 3.5 ~ 7, then to be mixed with the attapulgite deionized water suspension I of 10 ~ 50g/L by adding deionized water.
Preferably, the volume ratio of concentrated hydrochloric acid and mixed solution is 0 ~ 0.6:1, and the addition of concentrated hydrochloric acid does not get zero.
Preferably, time of repose is 0 ~ 24h, and time of repose does not get zero.
Preferably, the washing of pre-treatment step adopts the alternately washing of deionized water and absolute ethyl alcohol.
Compared with prior art, beneficial effect of the present invention shows:
1), the present invention adopts hydrolytic precipitation load method to prepare, and is that carrier is by accurate 1-dimention nano TiO with attapulgite
2particle is fixed and is formed stable TiO in its surface
2/ attapulgite photochemical catalyst.The nanoscale TiO of accurate one dimension pine needle shape pattern
2be distributed in uniform particles attapulgite on the surface, avoid TiO
2the reunion of particle, there will not be the TiO because reuniting effect causes
2the problem that the reduction of photochemical catalyst specific area and photocatalysis performance decline.TiO after calcination process
2/ attapulgite photochemical catalyst is that photodegradation rate reaches 98% under 10min ultraviolet lighting to the photocatalysis performance of methyl orange solution.
2), the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load of the present invention, be by a large amount of finely dispersed nanoscale TiO
2uniform particles is distributed in length and reaches the surface of hundreds of nanometer to the attapulgite of several microns, therefore under the prerequisite not needing extra equipment and energy ezpenditure, can realize the recovery of photochemical catalyst and reuse.
3), in hydrolytic precipitation process, by parameter adjustment, nanoscale TiO can be controlled
2the crystallite dimension of particle, Load Balanced and continuity.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of attapulgite.
Fig. 2 is TiO prepared by embodiment 1
2the transmission electron microscope photo TEM of/attapulgite photochemical catalyst.
Fig. 3 is TiO prepared by embodiment 2
2the transmission electron microscope photo TEM of/attapulgite photochemical catalyst.
Fig. 4 is TiO prepared by embodiment 3
2the transmission electron microscope photo TEM of/attapulgite photochemical catalyst.
Fig. 5 is TiO prepared by embodiment 3
2/ attapulgite photochemical catalyst under ultraviolet lighting to the absorbance curve of methyl orange solution.
Detailed description of the invention
For the ease of it will be appreciated by those skilled in the art that the present invention is further illustrated below in conjunction with accompanying drawing and embodiment.
Embodiment 1
1, preparing 50mL concentration is that 20g/L homodisperse attapulgite deionized water suspension I is in beaker.
Under the magnetic agitation condition of 2, ice-water bath and 200r/min, be the TiCl of 98% by 2.8ml concentration
4it is in the sulfuric acid solution of 20% that solution drops to 10ml concentration, and then adding deionized water preparation 250ml concentration is the TiCl of 0.1mol/L
4the aqueous solution.
3, be 2.5 by the pH value of suspension I described in 10% dilute sulfuric acid regulating step 1, beaker be placed in the water bath with thermostatic control of 85 DEG C, maintain the mechanical agitation of 300r/min, and add 20g urea as sustained release agent, obtain suspension II.
4, the 0.1mol/L TiCl described in step 2 is at the uniform velocity dripped with the speed of 1ml/min immediately
4the aqueous solution enters in the suspension II described in step 3, to TiCl
4continue at the mechanical agitation 30min maintaining 300r/min in the water bath with thermostatic control of 85 DEG C after the aqueous solution all drips, then by distilled water and absolute ethyl alcohol alternating centrifugal washing extremely neutrality, centrifugal recovery sediment is also drying to obtain TiO in 80 DEG C
2/ attapulgite photochemical catalyst.
TiO prepared by the present embodiment
2/ attapulgite photochemical catalyst is observed under the tem, discovery clearly can see the existence of pine needle shape titanium dioxide granule on concave convex rod, but titanium dioxide does not cover concave convex rod surface completely, the distribution of titanium dioxide granule on attapulgite discontinuous (as shown in Figure 2).
Embodiment 2
1, preparing 50mL concentration is 20g/L homodisperse attapulgite deionized water suspension, add 50mL concentrated hydrochloric acid (commercial grade concentration is the product of 37.5%) under agitation, leave standstill centrifugation after 12 hours and leave and take solid phase, it is 3.5 that gained solid phase deionized water and absolute ethyl alcohol are replaced washing to pH value, and is made into the homodisperse suspension I of concentration 20g/L by deionized water.
Under the magnetic agitation condition of 2, ice-water bath and 200r/min, be the TiCl of 98% by 2.8ml concentration
4it is in the sulfuric acid solution of 20% that solution drops to 10ml concentration, and then adding deionized water preparation 250ml concentration is the TiCl of 0.1mol/L
4the aqueous solution.
3, be 2.5 by the pH value of suspension I described in 10% dilute sulfuric acid regulating step 1, beaker be placed in the water bath with thermostatic control of 85 DEG C, maintain the mechanical agitation of 300r/min, and add 20g urea as sustained release agent, obtain suspension II.
4, the 0.1mol/L TiCl described in step 2 is at the uniform velocity dripped with the speed of 1ml/min immediately
4the aqueous solution enters in the suspension II described in step 3, to TiCl
4continue at the mechanical agitation 30min maintaining 300r/min in the water bath with thermostatic control of 85 DEG C after the aqueous solution all drips, then by distilled water and absolute ethyl alcohol alternating centrifugal washing extremely neutrality, centrifugal recovery sediment is also drying to obtain TiO in 80 DEG C
2/ attapulgite photochemical catalyst.
TiO prepared by the present embodiment
2/ attapulgite photochemical catalyst is observed under the tem, clearly can see that attapulgite covers one deck pine needle shape titanium dioxide granule on the surface equably, titanium dioxide granule being evenly distributed on attapulgite, soilless sticking (as shown in Figure 3).
Embodiment 3
1, preparing 50mL concentration is 20g/L homodisperse attapulgite deionized water suspension, add 50mL concentrated hydrochloric acid (commercial grade concentration is the product of 37.5%) under agitation, leave standstill centrifugation after 12 hours and leave and take solid phase, it is 4.5 that gained solid phase deionized water and absolute ethyl alcohol are replaced washing to pH value, and is made into the homodisperse suspension I of concentration 20g/L by deionized water.
Under the magnetic agitation condition of 2, ice-water bath and 200r/min, be the TiCl of 98% by 2.8ml concentration
4it is in the sulfuric acid solution of 20% that solution drops to 10ml concentration, and then adding deionized water preparation 250ml concentration is the TiCl of 0.1mol/L
4the aqueous solution.
3, be 2.5 by the pH value of suspension I described in 10% dilute sulfuric acid regulating step 1, beaker be placed in the water bath with thermostatic control of 85 DEG C, maintain the mechanical agitation of 300r/min, and add 20g urea as sustained release agent, obtain suspension II.
4, the 0.1mol/L TiCl described in step 2 is at the uniform velocity dripped with the speed of 1ml/min immediately
4the aqueous solution enters in the suspension II described in step 3, to TiCl
4the mechanical agitation 30min maintaining 300r/min in the water bath with thermostatic control of 85 DEG C is continued at after the aqueous solution all drips, then by distilled water and absolute ethyl alcohol alternating centrifugal washing extremely neutrality, centrifugal recovery sediment is in 80 DEG C of dryings again in 400 DEG C of roasting 1h, and obtaining take attapulgite as the accurate 1-dimention nano titanium dioxide composite photocatalyst of carrier.
TiO prepared by the present embodiment
2/ attapulgite photochemical catalyst is observed under the tem, clearly can see that attapulgite covers one deck pine needle shape titanium dioxide granule on the surface equably, titanium dioxide granule being evenly distributed on attapulgite, soilless sticking (as shown in Figure 4).
Fig. 5 is TiO prepared by this embodiment
2/ attapulgite photochemical catalyst under 10min ultraviolet lighting to the absorbance curve of methyl orange solution.
By formula D=(C
o-C)/C
o=(A
o-A)/A
o× 100% calculates its photodegradation rate reaches 98%.
In formula, D is photodegradation rate, C
o, C, A
o, A represents the concentration after the initial concentration of solution and decolouring, the absorbance after initial absorbance and decolouring respectively.
Above content is only to design example of the present invention and explanation; affiliated those skilled in the art make various amendment to described specific embodiment or supplement or adopt similar mode to substitute; only otherwise depart from the design of invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.
Claims (9)
1. the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load, is characterized in that, the carrier of this composite photo-catalyst is attapulgite, and the surface uniform of described attapulgite is distributed with the Nano titanium dioxide particle in pine needle pattern;
The preparation method of the accurate one-dimensional titanium dioxide composite photo-catalyst of above-mentioned attapulgite load, comprise hydrolytic precipitation load and the follow-up heat treatment process of nano titanium oxide, concrete steps are as follows:
1. 10 ~ 50g/L attapulgite deionized water suspension I, is prepared;
2., under the magnetic agitation condition of ice-water bath and 150 ~ 400r/min, be the TiCl of 98% by 2.5 ~ 7.0mL concentration
4it is in the sulfuric acid solution of 5 ~ 30% that solution drops to 10 ~ 30mL concentration, then adds the TiCl that deionized water compound concentration is 0.05 ~ 0.5mol/L
4the aqueous solution;
3., get 50 ~ 150mL suspension I and put into beaker, regulate suspension pH value to 2.0 ~ 3.5 with dilute sulfuric acid, beaker is placed in the water bath with thermostatic control of 80 ~ 90 DEG C, maintain the mechanical agitation of 150 ~ 400r/min, and add 15 ~ 25g sustained release agent, obtain suspension II;
4., with by TiCl
4the aqueous solution drops in suspension II, drips off rear continuation stirring 20 ~ 40min;
5., centrifugal recovery sediment, to wash to pH in neutral, collecting precipitation thing, obtains the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load through super-dry, roasting successively.
2. the preparation method of the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load according to claim 1, is characterized in that, step 3. middle sustained release agent is urea.
3. the preparation method of the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load according to claim 1, is characterized in that, step 4. middle rate of addition is 1mL/min.
4. the preparation method of the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load according to claim 1, is characterized in that, step 5. middle washing adopts the alternately washing of distilled water and absolute ethyl alcohol.
5. the preparation method of the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load according to claim 1, is characterized in that, step 5. middle baking temperature is 60 ~ 80 DEG C, and sintering temperature is 400 ~ 500 DEG C, and roasting time is 1 ~ 2h.
6. the preparation method of the accurate one-dimensional titanium dioxide composite photo-catalyst of the attapulgite load according to any one of Claims 1 to 5, it is characterized in that, preparation steps 1. described attapulgite deionized water suspension I time be also provided with attapulgite pre-treatment step, this pre-treatment step is specially: first prepare 10 ~ 50g/L attapulgite deionized water suspension, then add concentrated hydrochloric acid and obtain mixed solution, activate successively, leave standstill, centrifugal, washing to pH value is 3.5 ~ 7, the attapulgite deionized water suspension I of 10 ~ 50g/L is mixed with again by adding deionized water.
7. the preparation method of the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load according to claim 6, is characterized in that, the volume ratio of concentrated hydrochloric acid and mixed solution is 0 ~ 0.6:1, and the addition of concentrated hydrochloric acid does not get zero.
8. the preparation method of the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load according to claim 6, it is characterized in that, time of repose is 0 ~ 24h, and time of repose does not get zero.
9. the preparation method of the accurate one-dimensional titanium dioxide composite photo-catalyst of attapulgite load according to claim 6, is characterized in that, the washing of pre-treatment step adopts the alternately washing of deionized water and absolute ethyl alcohol.
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| CN106582590A (en) * | 2016-04-28 | 2017-04-26 | 北京华钛高科科技有限公司 | Glass fiber felt-nano TiO2 coating structure, preparation method therefor and use of glass fiber felt-nano TiO2 coating structure |
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| CN105906238B (en) * | 2016-04-25 | 2018-10-02 | 许宏俊 | A kind of health environment-friendly wall material and preparation method thereof |
| CN108355721B (en) * | 2018-02-02 | 2020-11-13 | 上海东化环境工程有限公司 | Modified carrier, supported catalyst and application thereof |
| CN108479778B (en) * | 2018-03-28 | 2020-11-24 | 常州大学 | Preparation method of modified attapulgite |
| CN108479777B (en) * | 2018-03-28 | 2020-11-24 | 常州大学 | Preparation method and application of attapulgite composite photocatalyst |
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| CN111545186A (en) * | 2020-05-14 | 2020-08-18 | 江西宝弘纳米科技有限公司 | Attapulgite loaded TiO2And preparation method and application thereof |
| CN112264069A (en) * | 2020-10-23 | 2021-01-26 | 南京信息工程大学 | Attapulgite photocatalyst and preparation method thereof |
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