CN103521270A - Sulfonated coal loaded TiO2 photocatalyst and preparation method thereof - Google Patents
Sulfonated coal loaded TiO2 photocatalyst and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a sulfonated coal loaded TiO2 photocatalyst and a preparation method thereof. A supported nanocrystal TiO2 photocatalyst taking semicoke sulfonated coal as a substrate is prepared through a microwave-liquid phase deposition method by taking high-polymer semi-organic matter sulfonated coal as a carrier and titanium sulfate as a titanium source, wherein the semicoke sulfonated coal as the carrier has the particle size of 0.15-0.3mm. The process comprises primary microwave radiation, centrifugal separation, multiple washing and suction filtration, secondary microwave radiation, ultrasonic wave washing and tertiary microwave radiation. The sulfonated coal loaded TiO2 photocatalyst prepared by the invention is better in adsorption property, high in photocatalytic performance, convenient to recycle, free of loss, incapable of weakening the photocatalytic performance, and suitable for wastewater treatment. The preparation method is simple in process, easy to operate, free of pollution and the like so as to be suitable for industrial production.
Description
Technical field
The invention belongs to semiconductor light-catalyst technical field, relate to a kind of sulfonated coal load TiO
2photochemical catalyst and preparation method thereof.
Background technology
Photocatalysis technology is a new environmental improvement technology, in wastewater degradation, have that energy consumption is low, easy and simple to handle, reaction condition is gentle, can reduce secondary pollution and can continued operation etc. advantage, receive much concern.TiO
2catalysis material is the current a kind of photochemical catalyst that has application potential most.TiO
2as durable photochemical catalyst, be used in and processed in various environmental problems.But current nanocrystal TiO
2not used on a large scale, is mainly because of its expensive cost, complicated preparation technology and the secondary pollution problems likely producing.
Current nano-TiO
2preparation method in be to adopt Muffle furnace high-temperature calcination mostly, and high-temperature calcination has following 2 deficiencies: the first, high-temperature calcination can promote nano-TiO
2transformation of crystal [
1] and strengthening crystal structure degree, but also easily cause crystal to reunite seriously and make nano-TiO
2it is large that the size of crystal grain becomes, and specific area is reduced.High degree of crystallinity is conducive to avoid the compound of electron-hole pair, and high specific area is conducive to adsorb the material that is degraded simultaneously, and both can improve nano-TiO
2photocatalysis efficiency
[2]but high-temperature calcination has improved degree of crystallinity and has but reduced specific area.The second, high-temperature calcination not only energy consumption is large, and has increased nano-TiO
2production cost, limited extensive investment application, but also limited the material (as organic polymers such as plastics, timber, PET) of some low thermal resistances as the use of load base material
[3].
For addressing the above problem, there are many scholars
[3-7]after deliberation prepare nano-TiO
2film.The preparation method of film is a lot, and such as liquid phase deposition, sol-gel process, chemical vapour deposition technique (CVD), thermal decomposition method, magnetron sputtering method etc., but the titanium source of film presoma is generally organic titanium source, has not only strengthened and has prepared nano-TiO
2cost, and in order to remove nano-TiO
2the organic matter of introducing in collosol suspension liquid preparation process, and reinforced nano TiO
2the fastness of load in substrate, conventionally need to be at more than 450 ℃ high temperature sinterings
[3], therefore in actual applications certain restriction nano-TiO
2large-scale production.
Traditional photocatalysis study general carries out in suspended state light-catalyzed reaction system.Because photochemical catalyst is present in reaction system with pulverous form, contact area is large, mass transfer effect good, so photocatalysis efficiency is higher.But the titanium dioxide granule that current business is used is tiny and proportion is less, make traditional filtration, precipitation, flocculation, the separation method such as centrifugal be difficult to photochemical catalyst to carry out separation, recovery and regeneration, and due to pulverous nano-TiO
2particle is easy to cohesion, free settling not in the aqueous solution, and catalyst is difficult to be recycled, and the loss of catalyst activity composition is large, the TiO of suspended state
2particle is on the absorption of light and stop the reasons such as the irradiation degree of depth that can affect light source, at present suspended state TiO
2photocatalytic system is mainly used in the research in laboratory, is difficult to carry out the commercial Application of scale, is unfavorable for circular regeneration and the recycling of catalyst
[8].At present a lot of research work are tended to photocatalyst fixation, both can solve the problem of separation and recovery of catalyst difficulty, can also overcome suspended phase poor catalyst stability and easy poisoning shortcoming
[9], and carry out on this basis improved process, to improving photocatalysis efficiency
[10-14].So S.X.Liu
[15]deng people, point out, the selection of carrier should at least meet following two conditions: the first, and nanocrystal TiO
2on carrier, there is good dispersive property, to improve light efficiency; The second, carrier should have good absorption property.
The present invention is from nano-TiO
2the problem existing in preparation and use procedure is set about, and in the whole preparation process of sample, without high-temperature calcination, adopting the preparation of microwave-liquid-phase precipitation method to take partly organic is the loaded nano crystal TiO of substrate
2photochemical catalyst, heating using microwave compares with traditional heating mode that to have firing rate fast, homogeneous heating, selectively heating, efficient energy-saving, is easy to control, cold sterilization, the feature such as pollution-free
[16], to solving above-mentioned existing problems.
TiO
2as photochemical catalyst, have very big development prospect, in recent years, how at low temperatures preparation has the anatase nanocrystal TiO of high catalytic activity
2become the focus of people's research.Current selected nano-TiO
2carrier mostly is inorganic matter, as: glass marble, iron oxide, aluminium oxide, diatomite, sepiolite etc.If can realize under low temperature and prepare nano-TiO
2, select organic matter or half organic matter to become possibility as carrier.Compare with inorganic matter, select the organic carrier that contains sulfonate ion can improve nano-TiO
2with the adhesion of carrier, it is more firmly loaded on carrier, thereby be difficult for appearing at, in degrading waste water process, there is the phenomenon that comes off.
Summary of the invention
Research of the present invention will be organized work for the problem of above two aspects, to the effect that: take semicoke brown coal as raw material, preparation has the sulfonated coal of certain mechanical strength; Utilize repeatedly microwave supplementary means, under cryogenic conditions, preparation has the highly active loaded nano crystal TiO that semicoke sulfonated coal is substrate of take
2photochemical catalyst; Provide that a kind of technique is simple, constant product quality, cost is lower, photocatalytic activity is higher supported titanium
2photochemical catalyst and preparation method thereof.
Technical scheme of the present invention is as follows:
A kind of sulfonated coal load TiO
2the preparation method of photochemical catalyst is to adopt the preparation of microwave-liquid-phase precipitation method to take the loaded nano crystal TiO that semicoke sulfonated coal is substrate
2photochemical catalyst; Semicoke sulfonated coal carrier granularity is 0.15mm～0.3mm.
The preparation method of catalyst of the present invention, the organic sulfonated coal of high polymer half of take is carrier, take titanium sulfate as titanium source, through microwave low temperature, be prepared from, comprise microwave, centrifugation, repeatedly wash suction filtration, secondary microwave radiation, ultrasonic washing and three microwaves.
The concrete steps of method of the present invention are as follows:
A. sulfonated coal is placed in one side through deionized water washing until water is clarified; The dilution heat of sulfuric acid that configuration solute is titanium sulfate, concentration is 0.1g/mL～0.2g/mL, to join in above-mentioned solution through the complete sulfonated coal of pretreatment, sulfonated coal and solution's solute mass ratio are in 1:(10～2.5), take alkaline solution in precipitating reagent adds above-mentioned solution until pH value is 5～6, mixed solution is put into and in microwave experiment stove, carried out one time microwave, heating using microwave 45min～75min under microwave power 390W～690W condition;
B. after a step microwave being completed, mixed liquor is put into 85 ℃～95 ℃ water bath with thermostatic control 9h～11h of constant temperature water bath;
C. centrifugation: the material after water bath with thermostatic control is carried out to Separation of Solid and Liquid, take off a layer solid;
D. first by deionized water sulfate ion in elimination reactant liquor after repeatedly washing suction filtration for the solid of c step separation, then use absolute ethanol washing;
E. secondary microwave radiation: the solid after suction filtration in d step is completed is placed on microwave experiment stove microwave power 390W～450W, radiated time 30min～60min radiation treatment;
F. ultrasonic washing: the drying solid that e step is obtained washs 20min～30min by deionized water under ultrasonic cleaner;
G. three microwaves: the TiO of the sulfonated coal load after f step has been washed
2under microwave power 390W～450W, radiant drying is processed 30min～40min.
Above-described carrier sulfonated coal is semicoke sulfonated coal.Described microwave experiment stove, comprises agitating device and condensation reflux unit.
Feature of the present invention and marked improvement are:
1. the sulfonated coal load TiO that prepared by the present invention
2photochemical catalyst has that good absorption property is good, photocatalysis performance is strong and be convenient to recycling, can not produce to run off and its photocatalysis performance can not weaken, and is applicable to wastewater treatment.
2. preparation method's operation of the present invention is simple, and easy operating is applicable to expand as suitability for industrialized production.
3. the present invention separately has that equipment requirement is simple, low temperature is prepared TiO
2do not need high-temperature roasting, preparation cost is lower, handling safety, the advantage such as pollution-free.
As Fig. 2 and Fig. 3, be sulfonated coal load TiO
2sEM and HRTEM phenogram, can find out nano-TiO
2be attached to uniformly sulfonated coal surface, TiO
2average grain diameter is 10nm.
As Fig. 4, be sulfonated coal load TiO
2xRD phenogram, adopt XRD method to measure photochemical catalyst and Myers computational methods show, the TiO of preparation
2crystal formation is single Detitanium-ore-type.According to Scherrer formula, calculate its average grain diameter and be about 10nm, substantially identical with HRTEM method measurement result.
Accompanying drawing explanation
Fig. 1: process flow diagram of the present invention;
Fig. 2: sulfonated coal load TiO
2sEM phenogram;
Fig. 3: sulfonated coal load TiO
2hRTEM phenogram;
Fig. 4: sulfonated coal load TiO
2xRD phenogram.
The specific embodiment
Embodiment 1
As shown in Figure 1, semicoke sulfonated coal load TiO
2preparation technology's flow process of photochemical catalyst mainly comprises: a microwave, water bath with thermostatic control, centrifugation, filtering and washing repeatedly, secondary microwave, ultrasonic washing, three microwaves.
Experimental procedure: by the 12g(semicoke sulfonated coal after washing and solution's solute mass ratio at 1:2.5) 0.15mm～0.3mm semicoke sulfonated coal adds in the pH=2 sulfuric acid solution (solution concentration is 0.1g/mL) that is dissolved with 30g titanium sulfate, fully stir, drip concentrated ammonia liquor to pH of mixed=5-6, after stirring, reactor is placed in after repacking with backflow, in the microwave experiment stove of agitating device, microwave 1h first under the condition of power P=530W, afterwards by reactor water bath with thermostatic control 11h at 90 ℃, centrifugation, deionized water, absolute ethanol washing suction filtration, gained filter cake is put into microwave experiment stove, dry 30min under the condition of microwave power P=390W, sample is through again using oscillation cleaning 30min under ultrasonic cleaner 100Hz after microwave treatment, suction filtration, filter cake is placed in to the dry 30min of microwave experiment stove that power is 420W, obtain sample.
Products obtained therefrom is sulfonated coal load TiO
2, be anatase, at catalyst concn, be 2.0g/L, the 15mg/L methylene blue solution of degrading under 365nm high voltage mercury lamp radiation, the degradation rate of 2h is 97.95%.
Embodiment 2
By the 3g(semicoke sulfonated coal after washing and solution's solute mass ratio at 1:10) 0.15mm～0.3mm semicoke sulfonated coal adds in the pH=2 sulfuric acid solution (solution concentration is 0.2g/L) that is dissolved with 30g titanium sulfate, fully stir, drip concentrated ammonia liquor to pH of mixed=5-6, after stirring, reactor is placed in after repacking with backflow, in the microwave experiment stove of agitating device, microwave 75min first under the condition of power P=690W, afterwards by reactor water bath with thermostatic control 10h at 95 ℃, centrifugation, deionized water, absolute ethanol washing suction filtration, gained filter cake is put into microwave experiment stove, dry 45min under the condition of microwave power P=450W, sample is through again using oscillation cleaning 20min under ultrasonic cleaner 100Hz after microwave treatment, suction filtration, filter cake is placed in to the dry 40min of microwave experiment stove that power is 390W, obtain sample.
Products obtained therefrom is sulfonated coal load TiO
2, be anatase, at catalyst concn, be 2.0g/L, the 15mg/L methylene blue solution of degrading under 365nm high voltage mercury lamp radiation, the degradation rate of 2h is 90%.
Embodiment 3
By the 12g(semicoke sulfonated coal after washing and solution's solute mass ratio at 1:2.5) 0.15mm～0.3mm semicoke sulfonated coal adds in the pH=2 sulfuric acid solution (solution concentration is 0.1g/mL) that is dissolved with 30g titanium sulfate, fully stir, drip concentrated ammonia liquor to pH of mixed=5-6, after stirring, reactor is placed in after repacking with backflow, in the microwave experiment stove of agitating device, microwave 1h first under the condition of power P=530W, afterwards by reactor water bath with thermostatic control 10h at 90 ℃, centrifugation, deionized water, absolute ethanol washing suction filtration, gained filter cake is put into microwave experiment stove, dry 45min under the condition of microwave power P=390W, sample is through again using oscillation cleaning 30min under ultrasonic cleaner 100Hz after microwave treatment, suction filtration, filter cake is placed in to the dry 30min of microwave experiment stove that power is 450W, obtain sample.
At catalyst concn, be 0.8g/L, 365nm high voltage mercury lamp radiation degraded 6mg/L methylene blue solution, reaction time 2h, used composite catalyst is reclaimed by filtration washing method, deionized water washing 2 times, after being dried to constant weight with 90 ℃, continue to use, repeat 6 degradation rates and be respectively 97.9%, 97.7%, 95.7%, 92%, 91.4%, 90.8%, in the process of recycling, find that half organic sulfonated coal carrier has certain mechanical strength, do not have, because of long-time stirring, broken phenomenon, half organic sulfonated coal load TiO occur
2photochemical catalyst has shown good stability.
Embodiment 4
By the 6g(semicoke sulfonated coal after washing and solution's solute mass ratio at 1:5) the semicoke sulfonated coal of 0.15mm～0.3mm adds in the pH=2 sulfuric acid solution that is dissolved with 30g titanium sulfate, fully stir, drip concentrated ammonia liquor to pH of mixed=5-6, after stirring, reactor is placed in after repacking with backflow, in the microwave experiment stove of agitating device, heating using microwave 1h first under the condition of power P=690W, afterwards by reactor water bath with thermostatic control 9h at 85 ℃, centrifugation, deionized water, absolute ethanol washing suction filtration, gained filter cake is put into microwave experiment stove, dry 30min under the condition of microwave power P=390W, sample after microwave treatment again with the clear 30min that vibrates under ultrasonic cleaning machine 100Hz, suction filtration, filter cake is placed in to the dry 40min of microwave experiment stove that power is 390W, obtain loaded photocatalyst sample.
Gained sample is sulfonated coal load TiO
2, be anatase, at catalyst concn, be 0.8g/L, the coking chemical waste water of the initial COD=333.3mg/L that degrades under 365nm high voltage mercury lamp radiation, reacts 2h under the condition that initial pH value is 8.7, coking chemical waste water COD degradation rate 83.64%.
The invention provides TiO
2effectively be carried on the technology on sulfonated coal surface, thoroughly to solve TiO
2loss in water treatment, difficult recovery problem.
List of references
[1] Zhang Liuxue, Wang Xiulian, low temperature is prepared photocatalytic nanometer titanium dioxide progress, functional material, 2007, supplementary issue 38:2376～2378
[2]T.Suprabha,Haizel?G.Roy,Jesty?Thomas,et?al.Microwave-Assisted?Synthesis?of?Titania?Nanocubes,Nanospheres?and?Nanorods?for?Photocatalytic?Dye?Degradation[J].Nanoscale?Research?Letter,2009,4:144～152.
[3]Ana?M.Peir,Jos?Peral,Concepcin?Domingo,etal.Low-Temperature?Deposition?of?TiO
2Thin?Films?with?Photocatalytic?Activity?from?Colloidal?Anatase?Aqueous?Solutions.Chem.Mater,2001,13(8):2567～2573.
[4]Guangshe?Li,Liping?Li,Juliana?Boerio-Goates,et?al.High?Purity?Anatase?TiO
2Nanocrystals--Near?Room?Temperature.ACS,2005,127(24):8659～8666.
[5] Peng Renyong, Lv Xinlian, highlight catalytic active anatase type nano TiO
2the low temperature preparation of colloidal sol, University Of Qingdao's journal,
2005,26(6):500～503.
[6] Zhou Xuedong, He Xin, Liu Baoshun etc., low temperature is prepared anatase TiO
2the colloidal sol aqueous solution, material Leader, 2005,19 (21): 65～67.
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2films?by?MePBIID.Nuclear?Instruments?and?Methods?in?Physics?Research?Section?B,2009,242(4):289～292.
[8] Zhang Yun, Zhao Lang, Yin Guangfu, Zhou great Li, Xu Xiujuan, titanic acid-sol legal system nano-TiO
2film and performance characterization, Chinese Journal of Inorganic Chemistry, 2004,8:991～995.
[9] Wu Sheng ，Tong bodyguard Tang, Liu Yali, TiO
2the type selecting of carrier of photocatalyst and carrying method research, Hunan Institute Of Engineering's journal,
2002,12(3):80～83.
[10]Watson?S,Beydoun?D,Amal?R.Synthesis?of?a?novel?magnetic?photocatalyst?by?direct?deposition?of?nanosized?crystals?onto?a?magnetic?core[J].Journal?of?Photochemistry?and?Photobiology?A:Chemistry,2002,148((1):303～313.
[11]Gao?Yuan,Chen?Baohua,Li?Hulin,et?al.Preparation?and?characterization?of?a?magnetically?separated?photocatalyst?and?its?catalytic?properties[J].Mater.Chem.Phys.,2003,80:348～355.
[12] Liu Ziquan, plateau, Jiang Fuyi, etc. different magnetic carriers are to the progress of magnet carried photocatalyst activity influence ［ J ］. modern chemical industry, 2008,28 (12): 25～27,29.
[13]Xu?Shihong,Shangguan?Wenfeng,Yuan?Jian,et?al.Preparations?and?photocatalytic?properties?of?magnetically?separable?nitrogen-doped?TiO
2supported?on?nickel?ferrite[J].Applied?Catalysis?B:Environmental,2006,71(3/4):177～184.
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2/AC?composite?photocatalyst?with?high?activity?and?easy?separation?prepared?by?a?hydrothermal?method.Journal?of?Hazardous?Materials,2007,143:p.257～263.
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Claims (5)
1. a sulfonated coal load TiO
2photochemical catalyst, is characterized in that take that semicoke sulfonated coal is as substrate, loaded with nano crystal TiO
2photochemical catalyst, semicoke sulfonated coal carrier granularity is 0.15mm～0.3mm.
2. the preparation method of the catalyst of claim 1, it is characterized in that take that the organic sulfonated coal of high polymer half is carrier, take titanium sulfate as titanium source, through microwave low temperature, be prepared from, comprise microwave, centrifugation, repeatedly wash suction filtration, secondary microwave radiation, ultrasonic washing and three microwaves.
3. method as claimed in claim 2, is characterized in that concrete steps are as follows:
A. sulfonated coal is placed in one side through deionized water washing until water is clarified; The dilution heat of sulfuric acid that configuration solute is titanium sulfate, concentration is 0.1g/mL～0.2g/mL, will join in above-mentioned solution through the complete sulfonated coal of pretreatment, sulfonated coal and solution's solute mass ratio are in 1:(10～2.5); Take alkaline solution in precipitating reagent adds above-mentioned solution until pH value is 5～6, mixed solution is put into and in microwave experiment stove, is carried out one time microwave, heating using microwave 45min～75min under microwave power 390W～690W condition;
B. after a step microwave being completed, mixed liquor is put into 85 ℃～95 ℃ water bath with thermostatic control 9h～11h of constant temperature water bath;
C. centrifugation: the material after water bath with thermostatic control is carried out to Separation of Solid and Liquid, take off a layer solid;
D. first by deionized water sulfate ion in elimination reactant liquor after repeatedly washing suction filtration for the solid of c step separation, then use absolute ethanol washing;
E. secondary microwave radiation: the solid after suction filtration in d step is completed is placed on microwave experiment stove microwave power 390W～450W, radiated time 30min～60min radiation treatment;
F. ultrasonic washing: the drying solid that e step is obtained washs 20min～30min by deionized water under ultrasonic cleaner;
G. three microwaves: the TiO of the sulfonated coal load after f step has been washed
2under microwave power 390W～450W, radiant drying is processed 30min～40min.
4. method as claimed in claim 3, is characterized in that described carrier sulfonated coal is semicoke sulfonated coal.
5. method as claimed in claim 3, is characterized in that described microwave experiment stove, comprises agitating device and condensation reflux unit.
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| CN108483786A (en) * | 2018-05-08 | 2018-09-04 | 陈少同 | A kind of emergency processing method of the sudden high strength ammonia polluted by nitrogen of water body |
| CN115228501A (en) * | 2022-08-24 | 2022-10-25 | 西安建筑科技大学 | Preparation and application of porous semi-coke activated carbon loaded ternary heterojunction photocatalyst |
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| CN105148890A (en) * | 2015-07-01 | 2015-12-16 | 龙岩学院 | Preparation method of coal cinder loaded nano-titanium dioxide composite material |
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| CN115228501A (en) * | 2022-08-24 | 2022-10-25 | 西安建筑科技大学 | Preparation and application of porous semi-coke activated carbon loaded ternary heterojunction photocatalyst |
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Application publication date: 20140122 |