CN104138752B - The process units of the compound silica aerogel photochemical catalyst of a kind of nano-titanium oxide and rare earth solid solution - Google Patents
The process units of the compound silica aerogel photochemical catalyst of a kind of nano-titanium oxide and rare earth solid solution Download PDFInfo
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- CN104138752B CN104138752B CN201410310857.3A CN201410310857A CN104138752B CN 104138752 B CN104138752 B CN 104138752B CN 201410310857 A CN201410310857 A CN 201410310857A CN 104138752 B CN104138752 B CN 104138752B
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Abstract
The invention discloses the process units of the compound silica aerogel photochemical catalyst of a kind of nano-titanium oxide and rare earth solid solution, it comprises the prefabricated tanks, gel still, aging sedimentation device, filter-press, solid solution set composite, spray dryer and the tubular type oscillation sintering furnace that are connected successively with entrance according to material outlet; Design and be applicable to industrialized process units according to preparation technology, solved the technical problem of the easy spontaneous formation aggregate of dichloride in anatase type level titanium oxide, reduced the production cost of finished product, be easy to realize industrialization.
Description
Technical field
The present invention relates to material technology field, particularly relate to a kind of nano-titanium oxide and rare earth solid solution is compoundThe process units of silica aerogel photochemical catalyst.
Background technology
Nano material is one of current international study hotspot and forward position. Owing to thering is not tool of macroscopic material instituteStandby small-size effect, surface and interface effect and quantum effect, nano material can show and conventional materialExpect distinct character (aspect such as optical, electrical, sound, heat, chemistry and mechanics), i.e. nano effect. Equally,For cellular solid, when porosity reaches after certain value, if hole dimension is enough little, also can showThe dimensional effect of portalling and skin effect, thus a series of properties that differ from conventional material produced. AirsettingGlue is the boundless novel nano porous material of a kind of application prospect. The wherein hole of aerosilGap rate can be up to 99.8%, and bore hole size is at 1～60nm, and specific area is up to 1000m2/ g, density can be 3～500kg/m3Between change. Utilize the high-specific surface area of aeroge can be used as adsorbent, practice shows, gasGel adsorber can have different shapes, size and chemical composition, and under different environmental conditions, absorption is cleanChange airborne pollution gas.
Nano titanium oxide is a kind of good catalysis material, and under illumination condition, titanium dioxide can make firstThe gas pollutants such as aldehyde, toluene, PM2.5 are converted into carbon dioxide and water, and pollutant is fundamentally given to lightSeparating and eliminate, is to eliminate one of effective method of atmosphere and indoor pollutant. Nano titanium dioxide photocatalysis materialThe problem that faces of material is mainly: 1, its crystalline phase must be the anatase titanium dioxide through high temperature sintering; 2, owing to receivingMeter level anatase titanium dioxide specific area is very large, and surface can be also very large, can spontaneous formation aggregate, and rawProduce cost very high, inconvenience is promoted the use of.
Application number is that 201210453899.3 patent of invention discloses a kind of metope with decomposing formaldehyde functionOrnament materials and preparation method thereof. That micro powder granule is bonded and fixed on decorative pattern layer specifically, micro-Powder particles comprises aerosil micro powder granule and nanometer titanium dioxide micropowder particle; Nano titanium oxideMicro powder granule with contacted by the air of formaldehyde pollution, and contact and catalytic reaction with formaldehyde, play purificationThe effect of room air. Its weak point is:
1, the component ratio of nano titanium oxide is little, and the effect purifying air is very limited;
2, nano titanium oxide cost is higher, and cost is high;
3, nano titanium oxide directly contacts with contaminated air, and it is surperficial without any safeguard measure, althoughCan carry out catalytic reaction with formaldehyde in a short time, but will soon occur " poisoning " phenomenon, thereby lose efficacy.
Summary of the invention
The object of the invention is for the technological deficiency existing in prior art, and a kind of nano-titanium oxide is providedWith the process units of the compound silica aerogel photochemical catalyst of rare earth solid solution, it can make dichloride in anatase type level oxygenChange the hole surface that titanium and rare earth solid solution are attached to silica aerogel equably, preparing can be long-acting, potentThe catalysis material of the gaseous contaminant such as formaldehyde, toluene in ground adsorption-decomposition function air.
For realizing the technical scheme that object of the present invention adopts be: a kind of nano-titanium oxide and rare earth solid solutionThe process units of compound silica aerogel photochemical catalyst, comprises be connected successively with entrance according to material outlet pre-Tank processed, gel still, aging sedimentation device, filter-press, solid solution set composite, spray dryer andTubular type oscillation sintering furnace.
Preferably, the power source of material transferring is preferably compressed-air actuated pressure, described prefabricated tanks gel still,Aging sedimentation device, filter-press and solid solution set composite are communicated to respectively compressed air generator.
Preferably, the material outlet of described solid solution set composite and the material inlet of described spray dryer itBetween slurry delivery pump is installed, this is because the slurry solid content in described solid solution set composite needs largeIn %, viscosity is higher, adopts the slurry delivery pump of larger power can make slurry enter smoothly described sprayingDrying machine is sprayed dry.
Described aging sedimentation device is two aging settling tanks that are arranged in parallel.
Described solid solution set composite is two compound stills of solid solution that are arranged in parallel.
In addition, described tubular type oscillation sintering furnace is connected with the water circulation cooling tank for cooling material, described waterCirculating cooling tank is connected with for collecting finished product and the cyclone separator that disperses hot blast, and described cyclone separator connectsBe connected to cloth bag separator; Described cloth bag separator is for separating and collect again finished product, and described cloth bag separatesDevice is connected with air-introduced machine, and described air-introduced machine is separated described cloth bag separator described in gas draws and pass intoThe cloth bag separator separation that circulates.
Concrete, described tubular type oscillation sintering furnace comprises the furnace foundation frame of body of heater and horizontal positioned; Described body of heaterInside be provided with boiler tube, described boiler tube and horizontal plane form the gradient of 5 °～8 °, described boiler tube is higherOne end is connected with hopper; One side of described body of heater is installed vibrating motor, the below of body of heater and described furnace foundationBetween frame, be provided with multiple rubber mats. Above-mentioned tubular type oscillation sintering furnace possesses vibrating function, and material existsAfter hopper enters, enter boiler tube, material along the gradient of boiler tube evenly forward, logical according to the time settingCross boiler tube.
Compared with prior art, the invention has the beneficial effects as follows: designed applicable industrialization according to preparation technologyProcess units, solved the technical problem of the easy spontaneous formation aggregate of dichloride in anatase type level titanium oxide, andTitanium oxide agglomeration traits is the main cause that causes preparation cost high; Prepared catalysis of the present inventionThe carrier of material is combined with active component firmly, adheres to that coated evenly photocatalysis performance is good, can be long-acting,The gaseous contaminants such as the airborne formaldehyde of potent adsorption-decomposition function, toluene, the more important thing is, the present invention producesInstall the fine problem that titanium oxide is reunited that solved, reduced the production cost of finished product, be easy to realize industrialization.
Brief description of the drawings
Figure 1 shows that the schematic diagram of process units of the present invention;
Figure 2 shows that the structural representation of tubular type oscillation sintering furnace.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail. Should be appreciated that described hereinSpecific embodiment only in order to explain the present invention, be not intended to limit the present invention.
Be illustrated in figure 1 process units schematic diagram of the present invention, it comprises according to material outlet and entrance and connecting successivelyThe prefabricated tanks 1, gel still 2, aging sedimentation device, filter-press 5, solid solution set composite, the spray that connectMist drying machine 9 and tubular type oscillation sintering furnace 10.
Preferably, the power source of material transferring is preferably compressed-air actuated pressure, described prefabricated tanks 1 gel still 2,Aging sedimentation device, filter-press 5 and solid solution set composite are communicated to respectively compressed air generator.
Preferably, the material outlet of described solid solution set composite and the material inlet of described spray dryer itBetween slurry delivery pump 8 is installed, this be because described solid solution set composite in slurry solid content need to be greater than40%, viscosity is higher, adopts the slurry delivery pump 8 of larger power can make slurry enter smoothly described sprayMist drying machine 9 is sprayed dry.
Described aging sedimentation device is two aging settling tanks 3,4 that are arranged in parallel.
Described solid solution set composite is the compound still 6,7 of two solid solution being arranged in parallel.
Described tubular type oscillation sintering furnace 10 is connected with the water circulation cooling tank 11 for cooling material, and described water followsRing cooling tank 11 is connected with for collecting finished product and the cyclone separator 12 that disperses hot blast, described cyclone separator12 are connected to cloth bag separator 13; Described cloth bag separator 13 is for separating again and collect finished product, instituteState cloth bag separator and be connected with air-introduced machine 14, described cloth bag separator 13 is separated gas by described air-introduced machineDraw and pass into the separation that circulates of described cloth bag separator 13.
Prefabricated tanks 1 is for mixing silica aerogel and ammoniacal liquor, and gel still 2 is for mixing titanium sulfate and deionized water,Solid solution set composite and aging sedimentation device are required consuming time longer in when work, arrange respectively two in parallelTwo compound stills 6,7 of solid solution and two aging settling tank 3,4 objects are to realize alternation, therebyRealizing serialization produces.
As shown in Figure 2, described tubular type oscillation sintering furnace 10 comprises the furnace foundation frame of body of heater 15 and horizontal positioned16; The inside of described body of heater 15 is provided with boiler tube 17, and described boiler tube 17 and horizontal plane form 5 °～8 °The gradient, the higher one end of described boiler tube 17 is connected with hopper 18; One side of described body of heater 15 is installed vibrationMotor 19, is provided with multiple rubber mats 20 between the below of body of heater 15 and described furnace foundation frame 16. OnThe tubular type oscillation sintering furnace 10 of stating possesses vibrating function, and material enters boiler tube 15 after hopper 18 enters,Material along the gradient of boiler tube 15 evenly forward, passes through boiler tube according to the time setting.
According to the production dress of above-mentioned a kind of nano-titanium oxide and the compound silica aerogel photochemical catalyst of rare earth solid solutionPut, its preparation method comprises the following steps:
(1) by silica aerogel particle through 300 mesh sieves, in prefabricated tanks 1, be soaked in 20 ° of ammoniacal liquor 30～36h, obtains expecting A; Rare earth nitrades is dissolved in deionized water with 1:1 weight ratio, after filtration, obtains expecting B;
(2) because scaling method and the standard of titanium sulfate in the time purchasing had nothing in common with each other, in order to add more accuratelyEnter the amount of titanium sulfate, the amount that is converted into titanium oxide taking titanium sulfate is demarcation means; Be converted into oxidation with titanium sulfateThe weight ratio of titanium counts 5%, in gel still 2, required titanium sulfate and weight ratio is counted to 95% deionizationWater is mixed and made into solution; Solution continued to stir and is heated to 75～90 DEG C, keep constant temperature, stirringMix when rotating speed is controlled at 500～800 revs/min and open ultrasonic vibration, in 60～90 minutes, at the uniform velocity addEnter the material A that step (1) is produced, these steps complete in gel still 2; The amount that adds pan feeding A be byThe weight of silica aerogel, the weight of silica aerogel is the weight that is converted into titanium oxide with titanium sulfate0.36～0.5 times;
(3) continue to add proper ammonia by pH value for being adjusted to 8.0～9.5, then aging settling tank (3,4) in, continue to stir with the mixing speed of 30～80 revs/min, when stirring, open ultrasonic vibration; Reaction60～90 minutes, obtain slurry C;
(4) by filter-press 5, slurry C is filtered, washed, the pH value of controlling slurry C is 7～8,Make the solid content of the slurry C after filtration, washing simultaneously > 40%; Then material is transferred to compound still (6,7),Add its deionized water of 2 times, add pan feeding B (the easy moisture absorption of rare earth nitrades can cause measuring inaccurate simultaneouslyReally, thus for the addition of accurate quantitative analysis rare earth nitrades, by rare earth nitrades in rare earth oxide),Wherein, material B middle rare earth nitrate is 3～7% of titania weight in the weight of oxide, speed of agitator controlBuilt in 500～800 revs/min, stir while being warming up to 75～90 DEG C, dripping ammoniacal liquor adjust pH is 7～7.5,Add hydrogen peroxide, the addition of hydrogen peroxide is material B middle rare earth nitrate in 10% of the weight of oxide, stirsMix reaction 30 minutes; Washing, filter after to material solid content > 40% time, collect and obtain slurry D;
At this moment, rare earth nitrades and ammoniacal liquor react and change rare-earth hydroxide into, and titanium sulfate and ammoniacal liquor are anti-Should generate titanium hydroxide; Rare-earth hydroxide is coated on the surface of titanium hydroxide, is jointly filled in silica aerogelSpecific surface on, the microcellular structure of silica aerogel the inside has been full of rare-earth hydroxide and titanium hydroxide; ProcessSpray after dry and high temperature sintering, rare-earth hydroxide changes rare earth oxide into, and titanium hydroxide changes oxygen intoChange titanium, its volume-diminished arrives original 0.2～0.4 times, makes silica aerogel again form microcellular structure; Rare earthThe zwitterion of hydroxide and titanium hydroxide is combined closely.
(5) will by slurry delivery pump by slurry D pump into spray dryer 9 spray dry, dry afterEnter tubular type oscillation sintering furnace 10, the heating-up temperature in tubular type oscillation sintering furnace is 450～600 DEG C, makes to be coatedTitanium hydroxide and rare-earth hydroxide on silica aerogel surface convert nano-scale anatase titanium oxide and rare earth toOxide, finally obtains nano-titanium oxide and rare earth oxide solid solution compound silica aerogel photochemical catalystFinished product.
In addition, described tubular type oscillation sintering furnace 10 is connected with the water circulation cooling tank 11 for cooling material, coldBut the material transferring after is extremely for collecting for the first time finished product and the cyclone separator 12 that disperses hot blast, described whirlwindSeparator 12 is connected to cloth bag separator 13; Described cloth bag separator 13 separates and collects for inferior for the second timeFinished product, described cloth bag separator is connected with air-introduced machine 14, and described air-introduced machine separates described cloth bag separator 13Out the separation that circulates of described cloth bag separator 13 is drawn and passed into gas.
Rare earth nitrades in above-mentioned steps (1) is lanthanum nitrate, cerous nitrate or neodymium nitrate.
In above-mentioned steps (2) or step (3), the frequency of ultrasonic vibration is 20～35KHz, and power density is 0.3～0.8W/cm2. Mixing while adopting ultrasonic vibration to make to stir is more even, promotes nano-scale particleFormation and do not reunite, can make clad material coated Si aeroge equably.
200～300 DEG C of the dry inlet temperatures of spraying used in above-mentioned steps (5), 100～120 DEG C of outlet temperatures.
In above-mentioned steps (5), the vibration frequency of tubular type oscillation sintering furnace is 300～380 beats/min.
Preparation principle of the present invention is: silica aerogel is considered to the solid of density minimum in the world, with traditionSorbing material compare, specific area is larger, has stronger adsorption capacity, is ideal catalystCarrier. Titanium oxide is prepared into rare-earth oxidation magnesium-titanium solid solution, on the one hand, makes titanium oxide there is higher catalysisActive; On the other hand, rare earth (lanthanum, cerium or neodymium) oxide makes nanoscale titanium oxide in relatively low temperatureThe lower relatively large anatase crystal type of realizing of degree transforms, and wherein the titanium oxide of part anatase crystal type changes rutile-type intoTitanium oxide. Nano-titanium oxide is attached on the specific surface of silica aerogel micropore, and silica aerogel is not only hadAbsorption catches the function of the gaseous contaminants such as formaldehyde in air, and can rely on the sharp titanium that is carried on its surfaceThe photocatalysis of type titanium oxide, decomposes the gaseous contaminant that is adsorbed seizure; The harmful gas of absorption when unglazedBody, has light time catalytic decomposition to discharge the innocuous gas and the moisture content that are converted; It is nano level to be that silica aerogel hasMicrocellular structure had carried out before one contaminated air before contaminated air contacts with nanoscale titanium oxideThe screening of phase, the micropore and the titanium oxide that make the pernicious gas such as formaldehyde, toluene and nanoscale enter silica aerogel are sent outRaw catalytic reaction, has avoided titanium oxide long term exposure that " poisoning " occurs in contaminated air and has caused inefficacySituation occurs; The present invention is by the screening function and the sharp titanium of nanoscale in early stage of the nano micropore structure capable of silica aerogelThe advantage of the catalysis of type titanium oxide rolls into one, and has realized long-actingization of this material catalysis and potentChange.
The above is only the preferred embodiment of the present invention, it should be pointed out that for the artThose of ordinary skill, under the premise without departing from the principles of the invention, can also make some improvement and profitDecorations, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. the process units of the compound silica aerogel photochemical catalyst of a nano-titanium oxide and rare earth solid solution, it is characterized in that, comprise the prefabricated tanks, gel still, aging sedimentation device, filter-press, solid solution set composite, spray dryer and the tubular type oscillation sintering furnace that are connected successively with entrance according to material outlet.
2. the process units of the compound silica aerogel photochemical catalyst of a kind of nano-titanium oxide according to claim 1 and rare earth solid solution, is characterized in that described prefabricated tanks, gel still, aging sedimentation device, filter-press and solid solution set composite are communicated to respectively compressed air generator.
3. the process units of the compound silica aerogel photochemical catalyst of a kind of nano-titanium oxide according to claim 1 and rare earth solid solution, is characterized in that, between the material outlet of described solid solution set composite and the material inlet of described spray dryer, slurry delivery pump is installed.
4. the process units of the compound silica aerogel photochemical catalyst of a kind of nano-titanium oxide according to claim 1 and 2 and rare earth solid solution, is characterized in that described aging sedimentation device is two aging settling tanks that are arranged in parallel.
5. according to the process units of a kind of nano-titanium oxide one of claim 1-3 Suo Shu and the compound silica aerogel photochemical catalyst of rare earth solid solution, it is characterized in that described solid solution set composite is two compound stills of solid solution that are arranged in parallel.
6. the process units of the compound silica aerogel photochemical catalyst of a kind of nano-titanium oxide according to claim 1 and rare earth solid solution, it is characterized in that described tubular type oscillation sintering furnace is connected with the water circulation cooling tank for cooling material, described water circulation cooling tank is connected with for collecting finished product and the cyclone separator that disperses hot blast, and described cyclone separator is connected to cloth bag separator.
7. the process units of the compound silica aerogel photochemical catalyst of a kind of nano-titanium oxide according to claim 1 and rare earth solid solution, is characterized in that described tubular type oscillation sintering furnace comprises the furnace foundation frame of body of heater and horizontal positioned; The inside of described body of heater is provided with boiler tube, and described boiler tube and horizontal plane form the gradient of 5 °～8 °, and one end that described boiler tube is higher is connected with hopper; One side of described body of heater is installed vibrating motor, between the below of body of heater and described furnace foundation frame, is provided with multiple rubber mats.
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| CN106179299B (en) * | 2016-06-24 | 2019-08-02 | 英鸿纳米科技股份有限公司 | Load the Preparation equipment of the aerogels of nano-titanium oxide |
| CN107282033B (en) * | 2017-06-28 | 2018-09-21 | 天津朗华科技发展有限公司 | A kind of photochemical catalyst and preparation method thereof for air V OC processing |
| CN107185515B (en) * | 2017-06-28 | 2018-09-25 | 郑善 | A kind of photochemical catalyst and preparation method thereof for sewage disposal |
| CN114984867A (en) * | 2022-08-03 | 2022-09-02 | 扬州晨化新材料股份有限公司 | Sectional type fixed bed reactor for catalyst production |
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Effective date of registration: 20170515 Address after: 300457, Tianjin economic and Technological Development Zone, No. 19 West Ring Road, TEDA Service Outsourcing Industrial Park, building 8, 2 floor Patentee after: Tianjin Long Hua Technology Development Co., Ltd. Address before: 300000 Tianjin City, Grand Port Fuyuan in 30-4-101 Patentee before: Cui Jiexin |
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