CN107670595A - A kind of Ga TiO2The preparation method of composite aerogel - Google Patents
A kind of Ga TiO2The preparation method of composite aerogel Download PDFInfo
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- CN107670595A CN107670595A CN201711058990.4A CN201711058990A CN107670595A CN 107670595 A CN107670595 A CN 107670595A CN 201711058990 A CN201711058990 A CN 201711058990A CN 107670595 A CN107670595 A CN 107670595A
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- tio
- composite aerogel
- preparation
- solution
- supercritical drying
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- 239000004964 aerogel Substances 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 43
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000000352 supercritical drying Methods 0.000 claims abstract description 20
- 239000011240 wet gel Substances 0.000 claims abstract description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- CHPZKNULDCNCBW-UHFFFAOYSA-N gallium nitrate Chemical compound [Ga+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CHPZKNULDCNCBW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 7
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 229940044658 gallium nitrate Drugs 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 39
- 238000006073 displacement reaction Methods 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 4
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000000845 anti-microbial effect Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 230000009102 absorption Effects 0.000 abstract 1
- 238000005352 clarification Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- 239000011259 mixed solution Substances 0.000 description 10
- 239000003292 glue Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 230000003115 biocidal effect Effects 0.000 description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 description 5
- 229910052733 gallium Inorganic materials 0.000 description 5
- -1 gallium nitrates Chemical class 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000013265 porous functional material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910021649 silver-doped titanium dioxide Inorganic materials 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Abstract
The present invention relates to a kind of Ga TiO2The preparation method of composite aerogel, by the way that butyl titanate, gallium nitrate, absolute ethyl alcohol, deionized water, nitric acid are stirred by certain mol proportion example, obtain the Ga TiO that solution is yellow clarification2Complex sol solution, stood in the baking oven of certain temperature and obtain wet gel for a period of time, processing is dried to wet gel using Supercritical Drying Technology and obtains Ga TiO2Composite aerogel, Ga TiO are obtained by grinding2Composite aerogel particle powder.The Ga TiO that the present invention prepares2Composite aerogel not only has the advantages that specific area, low-density, high porosity, and technical process is simple to operation, but also has excellent catalytic performance and anti-microbial property.Ga‑TiO2The preparation of composite aerogel, which is expected to gather around in fields such as antibacterial, photocatalysis and absorption, to have broad application prospects.
Description
Technical field
The invention belongs to the technical field of the composite porous preparation of inorganic nano, is related to a kind of Ga-TiO2Compound airsetting
The preparation method of glue, in particular by sol-gel process and the preparation method of Supercritical Drying Technology.
Background technology
TiO2Aeroge is a kind of novel nano porous functional material, has low-density, high-specific surface area, high catalytic activity
And the advantages that high adsorption activity.TiO will be utilized2The advantages that high surface area of aeroge and high adsorption activity, carries out compound with Ga Element
Ga-TiO is prepared2Composite aerogel, it can greatly improve TiO2Catalysis, adsorption activity and the anti-microbial property of aeroge, have
Hope applied to medical treatment, wastewater treatment and catalytic carrier etc..While one with being brought up in patent (CN106865605A)
Kind Ag-TiO2The preparation method of composite aerogel is compared, and noble metal is substituted using the raw material of the element containing Ga of relatively low cost
Ag, on the basis of anti-microbial property is ensured, it be able to can also not only be improved containing TiO while cost is reduced2Composite aerogel
Specific surface area, average pore size is less than 15nm.Therefore the Ga-TiO developed2The preparation method of composite aerogel is in catalysis, suction
Echoing antibacterial field has great development prospect.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, there is provided a kind of low cost, high-specific surface area and anti-
The Ga-TiO of bacterium excellent performance2The preparation method of composite aerogel.This method technique is simple to operation, and safety coefficient is high, can have
The increase TiO of effect2The anti-microbial property of aeroge.
The technical scheme is that：A kind of Ga-TiO2The preparation method of composite aerogel, it is comprised the following steps that：
(1) butyl titanate, absolute ethyl alcohol are mixed by certain mol proportion, is well mixed stirring, wiring solution-forming A；
(2) gallium nitrate, deionized water, nitric acid are mixed by certain mol proportion example, is well mixed stirring, wiring solution-forming B；
(3) step (2) solution B for being made into is added in the solution A into step (1), continuing stirring, to obtain clear yellow molten
Liquid；Wherein butyl titanate, absolute ethyl alcohol, gallium nitrate, deionized water, the mol ratio of nitric acid are 1：(15~30)：(0.01-
0.3)：(3~10)：(0.2~0.9)；
(4) yellow solution obtained in step (3) is poured into mould, is placed in isothermal reaction in baking oven and obtains Ga-TiO2
Compound wet gel；
(5) Ga-TiO obtained into step (4)2Compound wet gel adds organic solvent and carries out solvent displacement；
(6) by the Ga-TiO after being replaced in step (5)2Compound wet gel carries out supercritical drying processing, obtains Ga-TiO2
Composite aerogel；
(7) Ga-TiO that will be obtained in step (6)2Composite aerogel is ground, and obtains Ga-TiO2Composite aerogel
Grain.
Whipping temp is 15~35 DEG C in preferred steps (1), step (2) and step (3).
Stir speed (S.S.) is 350~650r/min in preferred steps (1), step (2) and step (3).
The temperature of baking oven is 35~60 DEG C in preferred steps (4)；The time of isothermal reaction is 0.5~3.5 hour.
Organic solvent is one kind of absolute ethyl alcohol, acetone or isopropyl acetone in preferred steps (5).
Solvent is replaced every 10~24 hours and changed once in preferred steps (5), is replaced 3~6 times altogether.
Supercritical drying described in preferred steps (6) is ethanol supercritical drying or CO2Supercritical drying.
It is preferred that above-mentioned ethanol supercritical drying parameter be kettle Stress control 7~10MPa, temperature control 265~
273 DEG C, the reaction time is 8~15 hours；CO2Supercritical drying parameter is kettle Stress control in 8~12MPa, temperature control
At 45~60 DEG C, drying time is 8~14 hours.
Beneficial effect：
(1) technique is simple to operation, excellent product performance.This method uses sol-gel process combination supercritical drying skill
Art prepares Ga-TiO2Composite aerogel, wherein sol-gel method craft are simple and easily repeat, and Supercritical Drying Technology can be prepared
Go out, the Ga-TiO of high-specific surface area uniform with hole2Composite aerogel.
(2) Ga-TiO that the present invention prepares2Composite aerogel not only has specific area, low-density, high porosity etc.
Advantage, but also can further improve catalytic performance and anti-microbial property.Ga-TiO2The preparation of composite aerogel is expected to anti-
The fields such as bacterium, photocatalysis and absorption, which are gathered around, to have broad application prospects.
Brief description of the drawings
Fig. 1 is Ga-TiO prepared by embodiment 12The photo in kind of aerogel composite；
Fig. 2 is Ga-TiO prepared by embodiment 12The SEM photograph of aerogel composite.
Embodiment
Example 1
1mol butyl titanates and 15mol absolute ethyl alcohols are well mixed stirring, stir speed (S.S.) 350r/ at 15 DEG C
Min, obtain TiO2Precursor solution A.0.015mol gallium nitrates, 4mol deionized waters and 0.2mol nitric acid are mixed at 15 DEG C
Uniform stirring, stir speed (S.S.) 350r/min, obtain settled solution B.Added to obtained mixed solution A in mixed solution B,
Continue to stir at 15 DEG C, stir speed (S.S.) 350r/min, obtain clear yellow solution.Obtained yellow solution is poured into mould
In, it is placed in isothermal reaction in 40 DEG C of baking ovens and obtains Ga-TiO in 3.5 hours2Compound wet gel.To obtained Ga-TiO2It is compound wet solidifying
Glue adds absolute ethyl alcohol and carries out solvent displacement, changes once within every 10 hours, replaces 3 times altogether.By the Ga-TiO after displacement2It is compound
Wet gel carries out ethanol supercritical drying processing, wherein kettle Stress control in 10MPa, temperature control at 270 DEG C, the reaction time
For 8 hours；Obtain Ga-TiO2Composite aerogel.The Ga-TiO that will be obtained2Composite aerogel is ground, and obtains Ga-TiO2It is multiple
Close aerogel particle.Obtained Ga-TiO2The photo in kind of composite aerogel particle is as shown in figure 1, be pale yellow powder shape.System
Standby Ga-TiO2The SEM photograph of aerogel composite is as shown in Fig. 2 aeroge even aperture distribution, average pore size are smaller.
Found by characterizing：Obtained Ga-TiO2Composite aerogel specific grain surface product is 275m2/ g, average pore size 13.2nm, 24 is small
When antibiotic rate 97.2%.
Example 2
1mol butyl titanates and 20mol absolute ethyl alcohols are well mixed stirring, stir speed (S.S.) 450r/ at 25 DEG C
Min, obtain TiO2Precursor solution A.0.1mol gallium nitrates, 6mol deionized waters and 0.4mol nitric acid are mixed at 25 DEG C
Even stirring, stir speed (S.S.) 450r/min, obtain settled solution B.Added to obtained mixed solution A in mixed solution B, 25
Continue to stir at DEG C, stir speed (S.S.) 450r/min, obtain clear yellow solution.Obtained yellow solution is poured into mould,
It is placed in isothermal reaction in 50 DEG C of baking ovens and obtains Ga-TiO in 2.5 hours2Compound wet gel.To obtained Ga-TiO2Compound wet gel adds
Enter acetone and carry out solvent displacement, change once within every 14 hours, replace 4 times altogether.By the Ga-TiO after displacement2Compound wet gel enters
Row CO2In 9MPa, temperature control at 48 DEG C, the reaction time is 10 hours for supercritical drying processing, wherein kettle Stress control；
To Ga-TiO2Composite aerogel.The Ga-TiO that will be obtained2Composite aerogel is ground, and obtains Ga-TiO2Composite aerogel
Grain.Found by characterizing：Obtained Ga-TiO2Composite aerogel specific grain surface product is 268m2/ g, average pore size 13.8nm, 24
Hour antibiotic rate 98.5%.
Example 3
1mol butyl titanates and 25mol absolute ethyl alcohols are well mixed stirring, stir speed (S.S.) 500r/ at 30 DEG C
Min, obtain TiO2Precursor solution A.0.2mol gallium nitrates, 8mol deionized waters and 0.6mol nitric acid are mixed at 30 DEG C
Even stirring, stir speed (S.S.) 500r/min, obtain settled solution B.Added to obtained mixed solution A in mixed solution B, 30
Continue to stir at DEG C, stir speed (S.S.) 500r/min, obtain clear yellow solution.Obtained yellow solution is poured into mould,
It is placed in isothermal reaction in 55 DEG C of baking ovens and obtains Ga-TiO in 2 hours2Compound wet gel.To obtained Ga-TiO2Compound wet gel adds
Absolute ethyl alcohol carries out solvent displacement, changes once within every 16 hours, replaces 5 times altogether.By the Ga-TiO after displacement2Compound wet gel
Ethanol supercritical drying processing is carried out, wherein for kettle Stress control in 8MPa, temperature control at 270 DEG C, the reaction time is 14 small
When；Obtain Ga-TiO2Composite aerogel.The Ga-TiO that will be obtained2Composite aerogel is ground, and obtains Ga-TiO2Compound airsetting
Glue particle.Found by characterizing：Obtained Ga-TiO2Composite aerogel specific grain surface product is 260m2/ g, average pore size
14.5nm, 24 hours antibiotic rates 99.1%.
Example 4
1mol butyl titanates and 28mol absolute ethyl alcohols are well mixed stirring, stir speed (S.S.) 550r/ at 35 DEG C
Min, obtain TiO2Precursor solution A.0.25mol gallium nitrates, 9mol deionized waters and 0.8mol nitric acid are mixed at 35 DEG C
Uniform stirring, stir speed (S.S.) 550r/min, obtain settled solution B.Added to obtained mixed solution A in mixed solution B,
Continue to stir at 35 DEG C, stir speed (S.S.) 550r/min, obtain clear yellow solution.Obtained yellow solution is poured into mould
In, it is placed in isothermal reaction in 55 DEG C of baking ovens and obtains Ga-TiO in 2 hours2Compound wet gel.To obtained Ga-TiO2Compound wet gel
Add isopropyl acetone and carry out solvent displacement, change once within every 24 hours, replace 5 times altogether.By the Ga-TiO after displacement2It is compound wet solidifying
Glue carries out CO2In 12MPa, temperature control at 55 DEG C, the reaction time is 12 small for supercritical drying processing, wherein kettle Stress control
When；Obtain Ga-TiO2Composite aerogel.The Ga-TiO that will be obtained2Composite aerogel is ground, and obtains Ga-TiO2Compound airsetting
Glue particle.Found by characterizing：Obtained Ga-TiO2Composite aerogel specific grain surface product is 255m2/ g, average pore size
14.3nm, 24 hours antibiotic rates 99.6%.
Example 5
1mol butyl titanates and 30mol absolute ethyl alcohols are well mixed stirring, stir speed (S.S.) 600r/ at 30 DEG C
Min, obtain TiO2Precursor solution A.0.3mol gallium nitrates, 10mol deionized waters and 0.9mol nitric acid are mixed at 30 DEG C
Uniform stirring, stir speed (S.S.) 600r/min, obtain settled solution B.Added to obtained mixed solution A in mixed solution B,
Continue to stir at 30 DEG C, stir speed (S.S.) 600r/min, obtain clear yellow solution.Obtained yellow solution is poured into mould
In, it is placed in isothermal reaction in 60 DEG C of baking ovens and obtains Ga-TiO in 1.5 hours2Compound wet gel.To obtained Ga-TiO2It is compound wet solidifying
Glue adds absolute ethyl alcohol and carries out solvent displacement, changes once within every 20 hours, replaces 6 times altogether.By the Ga-TiO after displacement2It is compound
Wet gel carries out ethanol supercritical drying processing, wherein kettle Stress control in 7MPa, temperature control at 265 DEG C, the reaction time
For 15 hours；Obtain Ga-TiO2Composite aerogel.The Ga-TiO that will be obtained2Composite aerogel is ground, and obtains Ga-TiO2It is multiple
Close aerogel particle.Found by characterizing：Obtained Ga-TiO2Composite aerogel specific grain surface product is 269m2/ g, average hole
Footpath 14.6nm, 24 hours antibiotic rates 99.3%.
Claims (8)
- A kind of 1. Ga-TiO2The preparation method of composite aerogel, it is comprised the following steps that：(1) butyl titanate, absolute ethyl alcohol are mixed by certain mol proportion, is well mixed stirring, wiring solution-forming A；(2) gallium nitrate, deionized water, nitric acid are mixed by certain mol proportion example, is well mixed stirring, wiring solution-forming B；(3) solution B that step (2) is made into is added in the solution A into step (1), continues stirring and obtains clear yellow solution；Its Middle butyl titanate, absolute ethyl alcohol, gallium nitrate, deionized water, the mol ratio of nitric acid are 1：(15~30)：(0.01-0.3)：(3 ~10)：(0.2~0.9)；(4) yellow solution obtained in step (3) is poured into mould, is placed in isothermal reaction in baking oven and obtains Ga-TiO2It is compound wet Gel；(5) Ga-TiO obtained into step (4)2Compound wet gel adds organic solvent and carries out solvent displacement；(6) by the Ga-TiO after being replaced in step (5)2Compound wet gel carries out supercritical drying processing, obtains Ga-TiO2It is compound Aeroge；(7) Ga-TiO that will be obtained in step (6)2Composite aerogel is ground, and obtains Ga-TiO2Composite aerogel particle.
- 2. preparation method according to claim 1, it is characterised in that stirring temperature in step (1), step (2) and step (3) Degree is 15~35 DEG C.
- 3. preparation method according to claim 1, it is characterised in that stirring speed in step (1), step (2) and step (3) Rate is 350~650r/min.
- 4. preparation method according to claim 1, it is characterised in that the temperature of baking oven is 35~60 DEG C in step (4)；It is permanent The time of temperature reaction is 0.5~3.5 hour.
- 5. preparation method according to claim 1, it is characterised in that organic solvent is absolute ethyl alcohol, acetone in step (5) Or one kind of isopropyl acetone.
- 6. preparation method according to claim 1, it is characterised in that solvent is replaced every 10~24 hours and changed in step (5) Once, replace 3~6 times altogether.
- 7. preparation method according to claim 1, it is characterised in that the supercritical drying described in step (6) surpasses for ethanol Critical drying or CO2Supercritical drying.
- 8. preparation method according to claim 7, it is characterised in that described ethanol supercritical drying parameter is kettle pressure In 7~10MPa, temperature control at 265~273 DEG C, the reaction time is 8~15 hours for power control；CO2Supercritical drying parameter is For kettle Stress control in 8~12MPa, temperature control at 45~60 DEG C, drying time is 8~14 hours.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111150877A (en) * | 2020-01-09 | 2020-05-15 | 军事科学院系统工程研究院卫勤保障技术研究所 | Mesoporous silicon nano-particles, preparation method and application |
| CN112831068A (en) * | 2021-03-02 | 2021-05-25 | 宁波福尔达智能科技有限公司 | Preparation method of novel antibacterial composite material |
| CN114054013A (en) * | 2021-12-03 | 2022-02-18 | 南京工业大学 | For CO2Photocatalytic reduced CeO2-TiO2Preparation method of composite aerogel |
| CN114108119A (en) * | 2020-08-25 | 2022-03-01 | 立肯诺(上海)新材料科技有限公司 | Antiviral pearl fiber and preparation method thereof |
| CN115634685A (en) * | 2022-11-03 | 2023-01-24 | 常熟理工学院 | Photocatalytic material responding to visible light and preparation method thereof |
| CN115646477A (en) * | 2022-10-14 | 2023-01-31 | 吉林大学 | Ga 0 /Ga 3+ -TiO 2 Composite photocatalyst and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111150877A (en) * | 2020-01-09 | 2020-05-15 | 军事科学院系统工程研究院卫勤保障技术研究所 | Mesoporous silicon nano-particles, preparation method and application |
| CN111150877B (en) * | 2020-01-09 | 2022-03-25 | 军事科学院系统工程研究院卫勤保障技术研究所 | Mesoporous silicon nano-particles, preparation method and application |
| CN114108119A (en) * | 2020-08-25 | 2022-03-01 | 立肯诺(上海)新材料科技有限公司 | Antiviral pearl fiber and preparation method thereof |
| CN112831068A (en) * | 2021-03-02 | 2021-05-25 | 宁波福尔达智能科技有限公司 | Preparation method of novel antibacterial composite material |
| CN114054013A (en) * | 2021-12-03 | 2022-02-18 | 南京工业大学 | For CO2Photocatalytic reduced CeO2-TiO2Preparation method of composite aerogel |
| CN115646477A (en) * | 2022-10-14 | 2023-01-31 | 吉林大学 | Ga 0 /Ga 3+ -TiO 2 Composite photocatalyst and preparation method thereof |
| CN115646477B (en) * | 2022-10-14 | 2024-01-26 | 吉林大学 | Ga (gallium) 0 /Ga 3+ -TiO 2 Composite photocatalyst and preparation method thereof |
| CN115634685A (en) * | 2022-11-03 | 2023-01-24 | 常熟理工学院 | Photocatalytic material responding to visible light and preparation method thereof |
| CN115634685B (en) * | 2022-11-03 | 2023-12-08 | 常熟理工学院 | Photocatalytic material responding to visible light and preparation method thereof |
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