CN109759047A - Preparation method of barium strontium titanate aerogel photocatalyst - Google Patents
Preparation method of barium strontium titanate aerogel photocatalyst Download PDFInfo
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- CN109759047A CN109759047A CN201910211282.2A CN201910211282A CN109759047A CN 109759047 A CN109759047 A CN 109759047A CN 201910211282 A CN201910211282 A CN 201910211282A CN 109759047 A CN109759047 A CN 109759047A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 239000004964 aerogel Substances 0.000 title claims abstract description 17
- 229910052454 barium strontium titanate Inorganic materials 0.000 title abstract 6
- 239000011941 photocatalyst Substances 0.000 title abstract 3
- 239000002105 nanoparticle Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 9
- WOIHABYNKOEWFG-UHFFFAOYSA-N [Sr].[Ba] Chemical compound [Sr].[Ba] WOIHABYNKOEWFG-UHFFFAOYSA-N 0.000 claims description 79
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 78
- 235000019441 ethanol Nutrition 0.000 claims description 36
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 29
- 229910052712 strontium Inorganic materials 0.000 claims description 28
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 28
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 27
- 230000032683 aging Effects 0.000 claims description 20
- 229910052788 barium Inorganic materials 0.000 claims description 20
- 239000011240 wet gel Substances 0.000 claims description 19
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000003607 modifier Substances 0.000 claims description 10
- 230000001476 alcoholic effect Effects 0.000 claims description 9
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 7
- 238000000352 supercritical drying Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 239000000499 gel Substances 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- NSXCBNDGHHHVKT-UHFFFAOYSA-N [Ti].[Sr].[Ba] Chemical compound [Ti].[Sr].[Ba] NSXCBNDGHHHVKT-UHFFFAOYSA-N 0.000 claims description 4
- -1 2- (2- methoxy ethoxy) acetic acid ethanol Chemical compound 0.000 claims description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims 2
- 238000009790 rate-determining step (RDS) Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 2
- 238000003911 water pollution Methods 0.000 abstract description 2
- 239000000975 dye Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 25
- 239000006228 supernatant Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
- 238000005070 sampling Methods 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 206010019909 Hernia Diseases 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 238000004817 gas chromatography Methods 0.000 description 4
- 239000013067 intermediate product Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000009963 fulling Methods 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- FDIKNXAYJUSCEO-UHFFFAOYSA-N [Sr].[Ba].CC(C)O Chemical compound [Sr].[Ba].CC(C)O FDIKNXAYJUSCEO-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- MTDMHAKNYZTKQR-UHFFFAOYSA-N [Ba][Ba] Chemical compound [Ba][Ba] MTDMHAKNYZTKQR-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- CDXSJGDDABYYJV-UHFFFAOYSA-N acetic acid;ethanol Chemical compound CCO.CC(O)=O CDXSJGDDABYYJV-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000010943 off-gassing Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a preparation method of a barium strontium titanate aerogel photocatalyst. The barium strontium titanate nano-particles are prepared by a hydrothermal method, then surface modification is carried out on the barium strontium titanate nano-particles, then the barium strontium titanate nano-particles are dispersed and gelled, and finally drying treatment is carried out. The barium strontium titanate aerogel powder prepared by the invention not only overcomes the problems of difficult recovery of the photocatalyst and secondary pollution to water, but also further improves the photocatalytic performance of the material. The prepared material has good stability, and can be used for treating water pollution caused by dyes in an environment-friendly way. The preparation method has the advantages of simple process, short reaction period and mass production prospect.
Description
Technical field:
The invention belongs to the preparation process fields of nano-porous materials, and in particular to a kind of barium strontium aeroge photocatalysis
The preparation method of agent.
Background technique:
Catalysis material nanosizing is one of the development trend of current catalysis material, and aeroge is because of its special three dimensional network
Network skeleton structure becomes a kind of emerging catalysis material.But the aerogels reported at present, major part is still
Some ingredients with photocatalytic activity are supported on the aeroge of bigger serface, and active constituent majority is in individual
Nanometer reunion state exists, not catalysis material truly.
Barium strontium is a kind of photochemical catalyst of common perovskite structure, in thermal stability, chemical stability and structure
All there is certain superiority in terms of stability, thus its catalytic activity is higher.Traditional barium strontium photochemical catalyst is mainly in powdery,
Powder obtained is easily reunited, and is easy moisture absorption in air and is occurred to go bad, and carried out at water using barium strontium powder
When reason, powder be will disperse in water body, is not easily recycled, and can cause secondary pollution to water body.By the perovskites substance such as barium strontium
It is prepared into Monolithic aerogel, is photocatalysis field urgent problem to be solved.
Summary of the invention:
A kind of barium strontium aeroge photocatalysis is provided the purpose of the invention is to improve the deficiencies in the prior art
The preparation method of agent, using Preparation of Metallic Strontium be barium source, barium metal is barium barium source, prepares barium strontium using nano particle construction from part
Aeroge has three-D nano-porous network structure, had not only improved the activity of aerogels, but also solve photochemical catalyst
The problem of being not easily recycled, and it is with good thermal stability, chemical stability, structural stability, its high-specific surface area
Its good adsorption effect is also gived, so being a kind of ideal catalysis material.
The technical solution of the present invention is as follows: a kind of preparation method of barium strontium aerogels, specific steps are such as
Under:
(1) preparation of strontium, barium source
It measures a certain amount of alcoholic solvent and is put into container, a certain amount of barium metal and Preparation of Metallic Strontium is added, in heating stirring to gold
Category is completely dissolved, and obtains strontium barium alcoholic solution；
(2) raw material mixes
A certain amount of titanium source is added in the strontium barium alcoholic solution of step (1), and continues to stir, forms strontium barium titanium mixed liquor；
(3) preparation of barium strontium nano particle
Strontium barium titanium mixed liquor obtained by step (2) is subjected to hydro-thermal reaction, nano particle is obtained, is put into baking oven and is dried,
Obtain barium strontium nano particle；
(4) surface of barium strontium nano particle is modified
Barium strontium nano particle is put into surface modifier solution and is stirred, n-hexane mixing is added, centrifugation obtains
By the modified barium strontium nano particle in surface；
(5) dispersion of barium strontium nano particle and gel
Ethanol solution will be added in modified nano particle made from step (4), add deionized water, is shaken through ultrasound
It after swinging, stands at a certain temperature, obtains barium strontium wet gel；
(6) aging and drying of barium strontium wet gel
Ageing solution is added in barium strontium wet gel made from step (5) and carries out aging, it is dry, obtain barium strontium airsetting
Glue.
It is preferred that above-mentioned alcoholic solvent is the mixture of one or both of benzyl alcohol or isopropanol.
Preparation of Metallic Strontium and the molar ratio of barium metal are 0.3~0.95 in preferred steps (1)；Preparation of Metallic Strontium, the quality of barium and alcohol are molten
The volume ratio of agent is 10~136.5g/L；The temperature heated in step (1) is 50~80 DEG C.
Titanium source used in preferred steps (2) is one of isopropyl titanate or butyl titanate；Titanium source and metal
Strontium, barium molar ratio be 1:(0.9~2.54)；The time persistently stirred is 10min-60min.
Hydrothermal temperature described in preferred steps (3) is 140~300 DEG C, and the reaction time is 24~96h；Baking oven
Temperature is 50 DEG C -80 DEG C.
Surface modifier in preferred steps (4) is 2- [2- (2- methoxy ethoxy) ethyoxyl] acetic acid or 2- (2- first
Oxygroup ethyoxyl) one of acetic acid ethanol solution；The concentration of surface modifier is 0.15~0.5mol/L；(individually below
Referred to as MEEAA solution and MEAA solution), the quality of barium strontium nano particle and the volume ratio of surface modifier solution are 20
~60g/L；It is 3h-5h that the time stirred after surface modifier solution, which is added,.
The volume ratio of n-hexane used in preferred steps (4) and surfactant solution is 3~10.
The fixing fabric structure that ethyl alcohol is added in preferred steps (5) is the matter of the barium strontium nano particle weighed in step (4)
Amount and the volume ratio of ethyl alcohol are 0.2~0.5g/L；The volume ratio of ethyl alcohol and deionized water is 0.5~5；Gelling temp is 25~65
℃。
Ageing solution described in preferred steps (6) is ethyl alcohol or deionized water；Ageing time is -72h for 24 hours, during which every 10-
14h replaces an Ageing solution；The drying means is freeze-drying, CO2In supercritical drying and ethanol supercritical drying
It is a kind of.
Barium strontium aerogel powder density obtained by the present invention is 0.08~0.30g/cm3, specific surface area 120.5~
185.5m2/g 10~50nm of average pore size.
The utility model has the advantages that
(1) it is compared to traditional photochemical catalyst, the barium strontium aeroge that the present invention is prepared is conducive in bulk
It is further to recycle, avoid secondary pollution.
(2) it is compared to the preparation process of traditional barium strontium photochemical catalyst, the present invention assembles legal system using nano particle
It is standby to can be prepared by barium strontium aerogels without heat treatment, it is easy to operate, and the sample stability produced is good, has
It hopes and realizes batch production.
(3) barium strontium aerogel powder produced by the present invention is used for water pollution control, can be recycled 7~8 times, green
Environmental protection.
Detailed description of the invention:
Fig. 1 is barium strontium aeroge XRD distribution map prepared by example 1.
Specific embodiment:
The present invention will be further explained below with reference to examples, but protection scope is not limited to this.
Example 1
0.4g Preparation of Metallic Strontium, 0.7g barium metal and 75mL benzyl alcohol are added in beaker, forms benzene first in 75 DEG C of stirring 80min
Alcohol strontium barium solution is cooled to room temperature to benzyl alcohol strontium barium solution, be added 2.78g isopropyl titanate (isopropyl titanate and Preparation of Metallic Strontium,
The molar ratio of barium is 1:0.9674), polytetrafluoroethyllining lining is poured into after stirring 30min, hydrothermal reaction kettle is put into, by hydro-thermal reaction
Kettle is put into chamber type electric resistance furnace, and 5 DEG C/min of heating rate is arranged, 200 DEG C of heat treatment temperature, handles time 48h, obtains barium strontium
Nano particle and supernatant liquor.Barium strontium nano particle and supernatant liquor are shaken up and all pour into centrifuge tube, is poured out after centrifugation
Clear liquid reuses ethanol washing three times, is put into 50 DEG C of baking oven drying.0.2g barium strontium nano particle is taken, being put into 5mL concentration is
The MEEAA solution of 0.3mol/L, stir 3h, pour into centrifuge tube, then into centrifuge tube be added 25mL n-hexane, after fulling shake from
The heart pours out supernatant liquor, takes out the modified barium strontium nano particle in surface, is loaded into sample bottle, then adds into sample bottle
Enter 0.5mL ethyl alcohol, magnetic agitation 10min adds 1mL deionized water, then ultrasonic vibration 5min, is put into 50 DEG C of baking ovens and stands
Gel obtains barium strontium wet gel.Ethyl alcohol is added into barium strontium wet gel and carries out aging, the amount of ethyl alcohol is overly moist solidifying not have
Subject to glue, ageing time 72h, during which every 12h replaces an ethyl alcohol.Barium strontium wet gel is put into reaction kettle and carries out ethyl alcohol
Supercritical drying, drying temperature are set as 270 DEG C, after temperature is gone up, and pressure maintains 12MPa, state under constant temperature and pressure
Lower maintenance 3h, then remains a constant speed and releases gas in 30min, takes out container after waiting temperature of reaction kettle to fall, obtains light
Catalysis barium strontium aerogel powder.Obtained density of material is
0.08g/cm3, specific surface area 150.27m2/ g, average pore size 20nm.Barium strontium aeroge prepared by this example
XRD distribution map generates required principal crystalline phase as shown in Figure 1, can be seen from the chart, without impurity phase, characteristic peak and standard card
Piece coincide good.Prepared blocky barium strontium aeroge is placed into the waste water for filling methyl blue, added with ultraviolet filter
It is irradiated under the hernia lamp of mating plate a hour, the observation of sampling in every ten minutes passes through uv-visible absorption spectra, gas-chromatography, liquid phase
Chromatography observes intermediate product and degradation effect to be changed less in five sub-samplings, and degradation effect is best, and repeats
It uses 8 times.
Example 2
0.85g barium metal and 0.23g Preparation of Metallic Strontium and 75mL benzyl alcohol are added in beaker, is formed in 50 DEG C of stirring 180min
Benzyl alcohol strontium barium solution is cooled to room temperature to benzyl alcohol strontium barium solution, 2.7g isopropyl titanate (isopropyl titanate and metal is added
Strontium, barium molar ratio be 1:0.9293), stir 30min after pour into polytetrafluoroethyllining lining, hydrothermal reaction kettle is put into, by hydro-thermal
Reaction kettle is put into chamber type electric resistance furnace, and 5 DEG C/min of heating rate is arranged, 250 DEG C of heat treatment temperature, handles time 72h, obtains metatitanic acid
Barium strontium nano particle and supernatant liquor.Barium strontium nano particle and supernatant liquor are shaken up and all pour into centrifuge tube, after centrifugation
Clear liquid is poured out, reuses ethanol washing three times, is put into baking oven and 60 DEG C of drying.0.5g barium strontium nano particle is taken, is put into
25mL concentration is the MEAA solution of 0.1mol/L, stirs 3h, pours into centrifuge tube, then 250mL n-hexane is added into centrifuge tube, is filled
It is centrifuged after point concussion, pours out supernatant liquor, take out the modified barium strontium nano particle in surface, be loaded into sample bottle, then to
1.5mL ethyl alcohol is added in sample bottle, magnetic agitation 10min adds 1mL deionized water, then ultrasonic vibration 5min, is put into 60
DEG C baking oven stands gel, obtains barium strontium wet gel.Ethyl alcohol is added into barium strontium wet gel and carries out aging, the amount of ethyl alcohol
It is subject to and does not cross wet gel, for 24 hours, during which every 10h replaces an ethyl alcohol to ageing time.Barium strontium aerogel precursor body is put into
CO is carried out in reaction kettle2Supercritical drying, drying temperature are set as 50 DEG C, and constant pressure 10MPa maintains 10h under certain outgassing rate,
After closing air inlet and discharging reacting kettle inner pressure, blocky barium strontium aeroge is obtained.Obtained density of material is
0.25g/cm3, specific surface area 127.4m2/ g, average pore size 11nm.Prepared blocky barium strontium aeroge is placed into Sheng
Have in the waste water of methyl orange, irradiated under the hernia lamp added with ultraviolet filter a hour, the observation of sampling in every ten minutes passes through purple
Outside-visible absorption spectra, gas-chromatography, liquid chromatogram are observed the drop in six sub-samplings to intermediate product and degradation effect
It is best to solve effect, and reusable 7 times.
Example 3
1g Preparation of Metallic Strontium and 2g barium metal and 40mL isopropanol are added in beaker, forms isopropanol in 80 DEG C of stirring 30min
Strontium barium solution is cooled to room temperature to isopropanol strontium barium solution, and 4.08g butyl titanate (isopropyl titanate and Preparation of Metallic Strontium, barium is added
Molar ratio be 1:1.81), stir 30min after pour into polytetrafluoroethyllining lining, be put into hydrothermal reaction kettle, hydrothermal reaction kettle put
Enter chamber type electric resistance furnace, 5 DEG C/min of heating rate is set, and 300 DEG C of heat treatment temperature, the processing time for 24 hours, obtains barium strontium nanometer
Particle and supernatant liquor.Barium strontium nano particle and supernatant liquor are shaken up and all pour into centrifuge tube, pours out clear liquid after centrifugation,
It reuses ethanol washing three times, is put into baking oven and 70 DEG C of drying.0.6g barium strontium nano particle is taken, being put into 10mL concentration is
The MEEAA solution of 0.2mol/L, stir 3h, pour into centrifuge tube, then into centrifuge tube be added 30mL n-hexane, after fulling shake from
The heart pours out supernatant liquor, takes out the modified barium strontium nano particle in surface, is loaded into sample bottle, then adds into sample bottle
Enter 2.4mL ethyl alcohol, magnetic agitation 10min adds 0.8mL deionized water, then ultrasonic vibration 5min, stands at 25 DEG C solidifying
Glue obtains barium strontium wet gel.Ethyl alcohol is added into barium strontium wet gel and carries out aging, the amount of ethyl alcohol is not to cross wet gel
Subject to, ageing time 48h, during which every 10h replaces an ethyl alcohol.Barium strontium aerogel precursor body is put into reaction kettle and is carried out
Ethanol supercritical drying, drying temperature are set as 250 DEG C, after temperature is gone up, and pressure maintains 10MPa, under constant temperature and pressure
2h is maintained under state, then remains a constant speed and releases gas in 30min, is taken out container after waiting temperature of reaction kettle to fall, is obtained
To blocky barium strontium aeroge.Obtained density of material is 0.13g/cm3, specific surface area 185.22m2/ g, average pore size
33nm.Prepared blocky barium strontium aeroge is placed into the waste water for filling rhodamine B, added with ultraviolet filter
It is irradiated under hernia lamp one and a half hours, the observation of sampling in every ten minutes passes through uv-visible absorption spectra, gas-chromatography, liquid chromatogram
It is best that the degradation effect in nine sub-samplings observed to intermediate product and degradation effect, and reusable 8 times.
Example 4
0.5g Preparation of Metallic Strontium, 1.2g barium metal, 10mL benzyl alcohol and 2.5mL isopropanol are added in beaker, is stirred at 60 DEG C
130min forms the mixed solution of benzyl alcohol strontium barium and isopropanol strontium barium, and solution to be mixed is cooled to room temperature, and 1.62g metatitanic acid is added
Isopropyl ester (isopropyl titanate is 1:2.53 with Preparation of Metallic Strontium, the molar ratio of barium), pours into polytetrafluoroethyllining lining after stirring 30min,
It is put into hydrothermal reaction kettle, hydrothermal reaction kettle is put into chamber type electric resistance furnace, 5 DEG C/min of heating rate, heat treatment temperature 150 are set
DEG C, time 96h is handled, barium strontium nano particle and supernatant liquor are obtained.Barium strontium nano particle is shaken with supernatant liquor
Even whole pours into centrifuge tube, pours out clear liquid after centrifugation, reuses ethanol washing three times, is put into baking oven and 80 DEG C of drying.Take 0.4g
Barium strontium nano particle is put into the MEAA solution that 10mL concentration is 0.5mol/L, stirs 3h, pour into centrifuge tube, then to centrifugation
70mL n-hexane is added in pipe, is centrifuged after fulling shake, pours out supernatant liquor, takes out the modified barium strontium nanometer in surface
Grain, is loaded into sample bottle, then 1.8mL ethyl alcohol is added into sample bottle, and magnetic agitation 10min adds 0.36mL deionization
Water, then ultrasonic vibration 5min, is put into 40 DEG C of baking ovens and stands gel, obtain barium strontium wet gel.To barium strontium wet gel
Middle addition ethyl alcohol carries out aging, and the amount of ethyl alcohol, which is subject to, does not cross wet gel, and ageing time 60h, during which every 12h replaces a second
Alcohol.Barium strontium wet gel is subjected to quenching using liquid nitrogen, then drying for 24 hours, obtains in the freeze drier of 50Pa
Photocatalysis barium strontium aerogel powder.Obtained density of material is 0.18g/cm3, specific surface area 168.3m2/ g, it is average
Aperture 25nm.Prepared blocky barium strontium aeroge is placed into the waste water for filling phenols, added with ultraviolet filter
Hernia lamp under irradiate one and a half hours, sampling in every ten minutes observation, pass through uv-visible absorption spectra, gas-chromatography, liquid phase color
It is best that spectrum is observed the degradation effect in nine sub-samplings to intermediate product and degradation effect, and reusable 7 times.
Claims (10)
1. a kind of preparation method of barium strontium aerogels, the specific steps of which are as follows:
(1) preparation of strontium, barium source
It measures a certain amount of alcoholic solvent and is put into container, a certain amount of barium metal and Preparation of Metallic Strontium is added, it is complete to metal in heating stirring
Fully dissolved obtains strontium barium alcoholic solution；
(2) raw material mixes
A certain amount of titanium source is added in the strontium barium alcoholic solution of step (1), and continues to stir, forms strontium barium titanium mixed liquor；
(3) preparation of barium strontium nano particle
Strontium barium titanium mixed liquor obtained by step (2) is subjected to hydro-thermal reaction, nano particle is obtained, is put into baking oven and is dried, obtained
Barium strontium nano particle；
(4) surface of barium strontium nano particle is modified
Barium strontium nano particle is put into surface modifier solution and is stirred, add n-hexane mixing, centrifugation, obtain by
The modified barium strontium nano particle in surface；
(5) dispersion of barium strontium nano particle and gel
Ethanol solution will be added in modified nano particle made from step (4), deionized water is added, through ultrasonic vibration
Afterwards, it stands at a certain temperature, obtains barium strontium wet gel；
(6) aging and drying of barium strontium wet gel
Ageing solution is added in barium strontium wet gel made from step (5) and carries out aging, it is dry, obtain barium strontium aeroge.
2. preparation method according to claim 1, it is characterised in that alcoholic solvent described in step (1) is benzyl alcohol or different
The mixture of one or both of propyl alcohol.
3. preparation method according to claim 1, it is characterised in that Preparation of Metallic Strontium and the molar ratio of barium metal are in step (1)
0.3~0.95；The volume ratio of Preparation of Metallic Strontium, the quality of barium and alcoholic solvent is 10~136.5g/L；The temperature of heating is in step (1)
50~80 DEG C.
4. preparation method according to claim 1, it is characterised in that titanium source used in step (2) is isopropyl titanate
Or one of butyl titanate；Titanium source and Preparation of Metallic Strontium, the molar ratio of barium are 1:(0.9~2.54)；The time persistently stirred is
10min-60min。
5. preparation method according to claim 1, it is characterised in that hydrothermal temperature described in step (3) is 140
~300 DEG C, the reaction time is 24~96h；The temperature of baking oven is 50 DEG C -80 DEG C.
6. preparation method according to claim 1, it is characterised in that the surface modifier in step (4) is 2- [2- (2- first
Oxygroup ethyoxyl) ethyoxyl] one of acetic acid or 2- (2- methoxy ethoxy) acetic acid ethanol solution；Surface modifier
Concentration is 0.15~0.5mol/L；The quality of barium strontium nano particle and the volume ratio of surface modifier solution are 20~60g/
L；It is 3h-5h that the time stirred after surface modifier solution, which is added,.
7. preparation method according to claim 1, it is characterised in that n-hexane and surfactant described in step (4)
The volume ratio of solution is 3~10.
8. preparation method according to claim 1, it is characterised in that the volume that ethyl alcohol is added in step (5) is rate-determining steps
(4) quality of the barium strontium nano particle weighed in and the volume ratio of ethyl alcohol are 0.2~0.5g/L；Ethyl alcohol and deionized water
Volume ratio is 0.5~5；Gelling temp is 25~65 DEG C.
9. preparation method according to claim 1, it is characterised in that Ageing solution described in step (6) be ethyl alcohol or go from
Sub- water；Ageing time is -72h for 24 hours, and during which every 10-14h replaces an Ageing solution；The drying means be freeze-drying,
CO2One of supercritical drying or ethanol supercritical drying.
10. preparation method according to claim 1, it is characterised in that barium strontium aerogel powder density obtained is
0.08~0.30g/cm3, 120.5~185.5m2/g of specific surface area, 10~50nm of average pore size.
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