CN106111112A - The preparation method of the aerogels of load nano-titanium oxide - Google Patents
The preparation method of the aerogels of load nano-titanium oxide Download PDFInfo
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Abstract
The invention provides the preparation method of a kind of aerogels loading nano-titanium oxide, the most previously prepared special pretreatment fluid, utilize the viscosity effect of Polyethylene Glycol in pretreatment fluid, in combination with Potassium Adipate, the complexation regulation effect of potassium citrate, the micropore loading titanium oxide making aeroge is more uniform；In pretreatment fluid mesotartaric acid potassium and reactant liquor, the product titanium dioxide that is combined into of potassium bicarbonate converts offer favourable conditions to anatase, in combination with the viscosity of potassium carbonate and peptizaiton and Potassium Adipate, the complexation regulation effect of potassium citrate, dispersibility and the covering power of reactant liquor can be improved, be more beneficial for product and be uniformly wrapped on aeroge micropore.The process of the present invention is relatively easy, it is easy to accomplish industrialization, and production cost is low.
Description
Technical field
The present invention relates to catalysis material technical field, a kind of aerogels loading nano-titanium oxide
Preparation method.
Background technology
Nano material is one of current international study hotspot and forward position.Little due to have not available for macroscopic material
Dimensional effect, surface and interfacial effect and quantum effect, nano material can show character distinct with conventional material
(aspect such as optical, electrical, sound, heat, chemistry and mechanics), i.e. nano effect.Equally, for cellular solid, work as porosity
After reaching certain value, if hole dimension is sufficiently small, also can show the dimensional effect portalled and skin effect, thus produce a series of different
Property in conventional material.Aeroge is the novel nano porous material that a kind of application prospect is boundless.Titanium dioxide
Silica aerogel has the network structure of mesoporous nano, has low-density, high-specific surface area and high porosity feature, therefore titanium dioxide
Silica aerogel has broad application prospects at aspects such as insulation, gas absorption and catalyst carriers.
Titanium dioxide has good photocatalytic activity, and under illumination condition, titanium dioxide can make formaldehyde, toluene, PM2.5
It is converted into carbon dioxide and water Deng gas pollutant, pollutant is fundamentally given photodissociation and eliminates, be to eliminate air and indoor
One of pollutant most efficient method.Simple nanometer titanium dioxide photocatalysis material problem encountered: one is that its crystalline phase must
It must be the anatase titanium dioxide through high temperature sintering；Two is due to nano-scale anatase titanium dioxide, and surface can be the biggest, it is possible to spontaneously forms
Aggregate, so its production cost is the highest, inconvenience is promoted the use of.
By titanium dioxide and aerosil compound preparation SiO2-TiO2Composite aerogel, it is possible to simultaneously play airsetting
The efficient absorption effect of plastic structure and the good photocatalysis performance of titanium dioxide.In prior art, have utilizes silicon dioxide gas
The method of gel micro powder granule and the mixing of nanometer titanium dioxide micropowder granule prepares SiO2-TiO2Micro powder granule, nanometer two therein
Titanium oxide fine powder granule contacts and catalytic reaction with formaldehyde, plays the effect purified the air of a room, column defects in the presence of it: one is
The component ratio of nano titanium oxide is little, and the effect purifying air is limited；Nano titanium oxide directly connects with contaminated air
Touch, its surface unprotect measure, easily occur " poisoning " phenomenon to lose efficacy.
In order to solve above-mentioned technical problem, nano oxidized titanium/rare earth is attached to aerosil by prior art
On specific surface, make silica aerogel not only have absorption and catch the function of the gaseous contaminants such as formaldehyde in air, and can rely on
It is carried on the photocatalysis of the anatase type titanium oxide on its surface, decomposes the adsorbed gaseous contaminant caught.But exist with
Lower problem: first, in solution, ammonia content is big, produces dangerous high；Secondly, its operation temperature is about 80 DEG C, and this makes molten
The ammonia volatilized in liquid is more, and production environment is more severe；Finally, the conversion of nano-scale anatase titanium oxide is at heating condition
Under carry out, switch condition is single, and conversion ratio is wayward, and gas photocatalysis effect needs to be improved further.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of aerogels loading nano-titanium oxide
Preparation method, solve that existing aerogels transformation of crystal rate is difficult to control to, production environment is severe, dangerous high
Problem.
The technical solution adopted for the present invention to solve the technical problems is: a kind of aeroge light loading nano-titanium oxide is urged
The preparation method of agent, comprises the following steps:
(1) preparation of pretreatment fluid: according to potassium hydroxide 1.9～2.3g/L, Soluble tartar. 20～24g/L, Potassium Adipate
3.8～5.6g/L, potassium citrate 3.6～5.1g/L, the standard preparation pretreatment fluid of butanol 33～95g/L, store for future use；
(2) take aerogel particles 160g, in the pretreatment fluid of the 1L being placed in 40～60 DEG C under stirring soak 24～
26h, obtains mixed liquor A；
(3) according to potassium bicarbonate 8～15g/L, the standard preparation reactant liquor of potassium carbonate 10～20g/L, at 40～60 DEG C
Adding mass concentration is the titanium sulfate solution of 5%, and the mass ratio between reactant liquor and titanium sulfate solution is 2～3:1, under stirring
Keep constant temperature 1～1.5 hours, obtain forerunner's reactant liquor；
(4) taking mixed liquor two parts, portion is mixed liquor A, and portion is mixed liquor B, and mixed liquor A is warming up to 100
～120 DEG C, mixed liquor B is warming up to 160～180 DEG C, and after intensification, stirring adds forerunner in two parts of mixed liquors simultaneously
Reactant liquor, opens supersonic vibration simultaneously, and mixed liquor A is 3～4:1 with the weight ratio of forerunner's reactant liquor, mixed liquor B and forerunner
The weight ratio of reactant liquor is 2～3:1, obtains slurry A and slurry B after reacting one hour respectively；
(5) slurry A and slurry B is added simultaneously in benzyl alcohol aqueous solution under stirring, is warming up to 200 DEG C, adds
Enter appropriate potassium hydroxide to regulate pH value to 10～11, start supersonic vibration, react 1.5～2 hours, obtain slurry C；
(6) slurry C being filtered, wash, the pH value controlling material C is 7～8, makes consolidating of the slurry C after filtration, washing simultaneously
Content > 40%；Then, adding its deionized water of 2 times, be simultaneously introduced rare earth nitrate, the addition of rare earth nitrate is slurry
The 10～12% of material C weight, are warming up to 80～90 DEG C, add hydrogen peroxide, and the addition of hydrogen peroxide is rare earth nitrate addition
6～8%, react 30 minutes；Washing, filter after to material solid content > 40% time, collect and obtain slurry D；
(7) slurry D is spray-dried, dried entrance tubular type oscillation sintering furnace, adding in tubular type oscillation sintering furnace
Hot temperature is 450～600 DEG C, the final aerogels obtaining described load nano-titanium oxide.
Preferably, in described benzyl alcohol aqueous solution, the volume ratio of benzyl alcohol and water is 2:3～5.
Preferably, described rare earth nitrate is Lanthanum (III) nitrate.
Preferably, the frequency of described supersonic vibration is 28～32KHz, and power density is 0.4～0.6W/cm2。
Preferably, the inlet temperature 240 of described spray drying～300 DEG C, outlet temperature 100～120 DEG C；Described tubular type is shaken
The angle of inclination swinging sintering furnace is 5～8 °, and vibration frequency is 300～380 beats/min.
Preferably, before adding rare earth nitrate, response system being applied magnetic field in step (6), magnetic direction is perpendicular to instead
Container, magnetic induction is answered to be preferably 1.2-2.5 tesla.
The positive effect of the present invention:
(1) previously prepared special pretreatment fluid in preparation technology, solves the production environment using ammonia to cause
Severe technical problem；What the pretreatment fluid of the present invention used is all potassium salt/alkali, and reaction effect is more preferable, poly-second in pretreatment fluid
Glycol plays certain viscosity effect, in combination with Potassium Adipate, the complexation regulation effect of potassium citrate, can make the micro-of aeroge
Hole loading titanium oxide is more uniform, and specific surface area is bigger, and reaches the effect extremely optimized, thus effective improves aeroge
Photocatalysis effect.
(2) in pretreatment fluid mesotartaric acid potassium of the present invention and reactant liquor potassium bicarbonate be combined into product titanium dioxide to sharp
Titanium ore converts provides favourable conditions, in combination with the viscosity of potassium carbonate and peptizaiton and Potassium Adipate, the complexation of potassium citrate
Regulation effect, can improve dispersibility and the covering power of reactant liquor, is more beneficial for product and is uniformly wrapped on aeroge micropore.
Secondary hydrothermal treatment consists in the mixing of different temperatures mixed liquor simultaneously and benzyl alcohol aqueous solution achieves product
In thing titanium dioxide, anatase and the content of brockite and the further of pattern control, so that brockite and anatase reach
Optimal proportion, to show the highest photocatalytic activity.
(3) addition and the course of reaction of rare earth nitrate is carried out under the existence condition of magnetic field, under conditions of externally-applied magnetic field,
The magnetohydrodynamics effect that Lorentz force causes has interfered significantly on course of reaction, meeting during ion stream cutting magnetic line in solution
Acted on by Lorentz force；Lorentz force makes ion make helix directed movement, thus serves the stirring action for the treatment of fluid,
And make ion make orientation accelerated motion, the beneficially rare earth oxide uniform cladding at aeroge micropore, time promote that enhancing is received
The catalysis activity of rice titanium oxide.
(4) process of the present invention is relatively easy, it is easy to accomplish industrialization, at the bottom of production cost.
Detailed description of the invention
Below to a preferred embodiment of the present invention will be described in detail.
Embodiment 1
The preferred embodiment of the present invention provides the preparation method of a kind of aerogels loading nano-titanium oxide, including
Following steps:
(1) preparation of pretreatment fluid: according to potassium hydroxide 1.9～2.3g/L, Soluble tartar. 20～24g/L, Potassium Adipate
3.8～5.6g/L, potassium citrate 3.6～5.1g/L, the standard preparation pretreatment fluid of butanol 33～95g/L, store for future use；
(2) take aerogel particles 160g, in the pretreatment fluid of the 1L being placed in 40～60 DEG C under stirring soak 24～
26h, obtains mixed liquor A；
(3) according to potassium bicarbonate 8～15g/L, the standard preparation reactant liquor of potassium carbonate 10～20g/L, at 40～60 DEG C
Adding mass concentration is the titanium sulfate solution of 5%, and the mass ratio between reactant liquor and titanium sulfate solution is 2～3:1, under stirring
Keep constant temperature 1～1.5 hours, obtain forerunner's reactant liquor；
(4) taking mixed liquor two parts, portion is mixed liquor A, and portion is mixed liquor B, and mixed liquor A is warming up to 100
～120 DEG C, mixed liquor B is warming up to 160～180 DEG C, and after intensification, stirring adds forerunner in two parts of mixed liquors simultaneously
Reactant liquor, opens supersonic vibration simultaneously, and mixed liquor A is 3～4:1 with the weight ratio of forerunner's reactant liquor, mixed liquor B and forerunner
The weight ratio of reactant liquor is 2～3:1, obtains slurry A and slurry B after reacting one hour respectively；
(5) slurry A and slurry B is added simultaneously in benzyl alcohol aqueous solution under stirring, is warming up to 200 DEG C, adds
Enter appropriate potassium hydroxide to regulate pH value to 10～11, start supersonic vibration, react 1.5～2 hours, obtain slurry C；
(6) slurry C being filtered, wash, the pH value controlling material C is 7～8, makes consolidating of the slurry C after filtration, washing simultaneously
Content > 40%；Then, adding its deionized water of 2 times, be simultaneously introduced rare earth nitrate, the addition of rare earth nitrate is slurry
The 10～12% of material C weight, are warming up to 80～90 DEG C, add hydrogen peroxide, and the addition of hydrogen peroxide is rare earth nitrate addition
6～8%, react 30 minutes；Washing, filter after to material solid content > 40% time, collect and obtain slurry D；
(7) slurry D is spray-dried, dried entrance tubular type oscillation sintering furnace, adding in tubular type oscillation sintering furnace
Hot temperature is 450～600 DEG C, the final aerogels obtaining described load nano-titanium oxide.
In described benzyl alcohol aqueous solution, benzyl alcohol is 2:3～5 with the volume ratio of water.
Described rare earth nitrate is Lanthanum (III) nitrate.
The frequency of described supersonic vibration is 28～32KHz, and power density is 0.4～0.6W/cm2。
The inlet temperature 240 of described spray drying～300 DEG C, outlet temperature 100～120 DEG C；Described tubular type vibration sintering
The angle of inclination of stove is 5～8 °, and vibration frequency is 300～380 beats/min.
Before adding rare earth nitrate in step (6), response system being applied magnetic field, magnetic direction is perpendicular to reaction vessel,
Magnetic induction is preferably 1.2-2.5 tesla.
Comparative example
The preparation method of a kind of aerogels loading nano-titanium oxide, comprises the following steps:
(1) aerogel particles is through 300 mesh sieves, is soaked in 36h in 20 ° of ammonia, is referred to as material A standby, by Lanthanum (III) nitrate with 1:1
Weight ratio is dissolved in deionized water, and after filtration, standby being referred to as expects B；
(2) by titanium sulfate weight ratio 28kg (content of titanium dioxide in titanium sulfate is 20%) and deionized water 500kg
Mixed solution, is heated to 78 DEG C while stirring, keeps constant temperature, and speed of agitator controls to open Under Ultrasonic Vibration while 680 revs/min
Dynamic, frequency F of supersonic vibration is 35KHz, and power density P is 0.3W/cm2, at the uniform velocity adds silica aerogel (material A) in 68 minutes
4.3kg, reacts 20min after adding；
(3) proper ammonia (concentration is 20%) is added by the pH value of system for regulating to 8.5, then with 50 revs/min
Mixing speed stirs, and opens supersonic vibration while stirring；React 70 minutes, obtain slurry C；
(4) slurry C being filtered, wash, the pH value making slurry C is 7.8, after filter material solid content 45%；Add 300kg
Deionized water, is simultaneously introduced the material B of 0.25kg, and speed of agitator controls at 700 revs/min, when stirring is warming up to 78 DEG C, sprays ammonification
Water adjusts pH value 7.5, adds hydrogen peroxide 25ml, stirring reaction 30 minutes；Washing, filtration, material solid content 42%, obtain slurry D；
(5) slurry D is spray-dried, is dried inlet temperature 280 DEG C, outlet temperature 110 DEG C.Shake subsequently into tubular type
Swinging stove, in stove, heating-up temperature is set to 480 DEG C, makes the titanium hydroxide/lanthanum being coated on aeroge surface be converted into nano-scale anatase
Titanium oxide/lanthanum, finally gives the silica aerogel photocatalyst that nano-titanium oxide/lanthanum solid solution is compound.
In embodiment 1 and comparative example, aerogel particles is purchased from nano high-tech company limited of Shaoxin City, and its specific surface area reaches
600m2/ g, through entrusting third party (SGS company) to measure, embodiment 1 is as follows with the index preparing finished product of comparative example:
From data, the silica aerogel photocatalyst mean diameter of embodiment 1 gained load nano-titanium oxide reaches
Below 20nm, its specific surface area has reached 350m especially2About/g, the product containing 13% brockite and 82% anatase shows
The highest photocatalytic activity and Degradation Formaldehyde rate.As can be seen here, the aerogels that prepared by the present invention has higher ratio
Surface area, absorbability is higher so that it is catalytic performance is higher.
Above-described only the preferred embodiments of the present invention, the explanation of it should be understood that above example is simply used
In helping to understand method and the core concept thereof of the present invention, the protection domain being not intended to limit the present invention, all the present invention's
Any amendment of being made within thought and principle, equivalent etc., should be included within the scope of the present invention.
Claims (7)
1. the preparation method of the aerogels loading nano-titanium oxide, it is characterised in that comprise the following steps:
(1) preparation of pretreatment fluid: according to potassium hydroxide 1.9～2.3g/L, Soluble tartar. 20～24g/L, Potassium Adipate 3.8～
5.6g/L, potassium citrate 3.6～5.1g/L, the standard preparation pretreatment fluid of butanol 33～95g/L, store for future use；
(2) take aerogel particles 160g, the pretreatment fluid of the 1L being placed in 40～60 DEG C soak under stirring 24～26h,
Obtain mixed liquor A；
(3) according to potassium bicarbonate 8～15g/L, the standard preparation reactant liquor of potassium carbonate 10～20g/L, add at 40～60 DEG C
Mass concentration is the titanium sulfate solution of 5%, and the mass ratio between reactant liquor and titanium sulfate solution is 2～3:1, keeps under stirring
Constant temperature 1～1.5 hours, obtain forerunner's reactant liquor；
(4) taking mixed liquor two parts, portion is mixed liquor A, and portion is mixed liquor B, and mixed liquor A is warming up to 100～120
DEG C, mixed liquor B is warming up to 160～180 DEG C, and after intensification, stirring adds forerunner's reaction in two parts of mixed liquors simultaneously
Liquid, opens supersonic vibration simultaneously, and mixed liquor A is 3～4:1 with the weight ratio of forerunner's reactant liquor, and mixed liquor B reacts with forerunner
The weight ratio of liquid is 2～3:1, obtains slurry A and slurry B after reacting one hour respectively；
(5) slurry A and slurry B is added simultaneously in benzyl alcohol aqueous solution under stirring, is warming up to 200 DEG C, add suitable
PH value is regulated to 10～11 by amount potassium hydroxide, starts supersonic vibration, reacts 1.5～2 hours, obtain slurry C；
(6) slurry C being filtered, wash, the pH value controlling material C is 7～8, makes the solid content of the slurry C after filtration, washing simultaneously >
40%；Then, adding its deionized water of 2 times, be simultaneously introduced rare earth nitrate, the addition of rare earth nitrate is slurry C weight
Amount 10～12%, be warming up to 80～90 DEG C, add hydrogen peroxide, the addition of hydrogen peroxide be rare earth nitrate addition 6～
8%, react 30 minutes；Washing, filter after to material solid content > 40% time, collect and obtain slurry D；
(7) slurry D is spray-dried, dried entrance tubular type oscillation sintering furnace, the heating temperature in tubular type oscillation sintering furnace
Degree is 450～600 DEG C, the final aerogels obtaining described load nano-titanium oxide.
The preparation method of a kind of aerogels loading nano-titanium oxide the most according to claim 1, its feature
It is: in described benzyl alcohol aqueous solution, benzyl alcohol is 2:3～5 with the volume ratio of water.
The preparation method of a kind of aerogels loading nano-titanium oxide the most according to claim 1, its feature
It is: described rare earth nitrate is Lanthanum (III) nitrate.
The preparation method of a kind of aerogels loading nano-titanium oxide the most according to claim 1, its feature
Being: the frequency of described supersonic vibration is 28～32KHz, power density is 0.4～0.6W/cm2。
The preparation method of a kind of aerogels loading nano-titanium oxide the most according to claim 1, its feature
It is: the inlet temperature 240 of described spray drying～300 DEG C, outlet temperature 100～120 DEG C；Described tubular type oscillation sintering furnace
Angle of inclination is 5～8 °, and vibration frequency is 300～380 beats/min.
The preparation method of a kind of aerogels loading nano-titanium oxide the most according to claim 1, its feature
It is: before adding rare earth nitrate in step (6), response system being applied magnetic field, magnetic direction is perpendicular to reaction vessel.
The preparation method of a kind of aerogels loading nano-titanium oxide the most according to claim 6, its feature
It is: magnetic induction is preferably 1.2-2.5 tesla.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107185515A (en) * | 2017-06-28 | 2017-09-22 | 郑善 | It is a kind of for photochemical catalyst of sewage disposal and preparation method thereof |
| CN107245230A (en) * | 2017-06-28 | 2017-10-13 | 郑善 | A kind of PET polyester slices with air-cleaning function and its preparation method and application |
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| CN101522565A (en) * | 2006-10-13 | 2009-09-02 | 赢创德固赛有限责任公司 | Surface-modified silicas |
| US20100316561A1 (en) * | 2008-02-11 | 2010-12-16 | Daunia Solar Cell S.R.L. | Process for the preparation of titanium dioxide with nanometric dimensions and controlled shape |
| CN104056616A (en) * | 2014-07-01 | 2014-09-24 | 崔洁心 | Method for preparing silica aerogel photocatalyst formed by compounding nanometer titanium oxide and rare earth solid solution |
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| CN1830565A (en) * | 2006-04-20 | 2006-09-13 | 复旦大学 | Synthesis method of nanometer crystal mesopore titanium dioxide photocatalyst |
| CN101522565A (en) * | 2006-10-13 | 2009-09-02 | 赢创德固赛有限责任公司 | Surface-modified silicas |
| US20100316561A1 (en) * | 2008-02-11 | 2010-12-16 | Daunia Solar Cell S.R.L. | Process for the preparation of titanium dioxide with nanometric dimensions and controlled shape |
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| CN107185515A (en) * | 2017-06-28 | 2017-09-22 | 郑善 | It is a kind of for photochemical catalyst of sewage disposal and preparation method thereof |
| CN107245230A (en) * | 2017-06-28 | 2017-10-13 | 郑善 | A kind of PET polyester slices with air-cleaning function and its preparation method and application |
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Effective date of registration: 20181228 Address after: 301707 Block 103-10 (Centralized Office District), East Side Development Center, Zhongji Road, Douzhangzhuang Township, Wuqing District, Tianjin Patentee after: Anglo nanoscale Polytron Technologies Inc Address before: 300381 C-2-202, Nankai District, Tianjin. Patentee before: Cui Jianzhong |