CN107626305A - A kind of synthetic method of plasma photocatalysis agent and application - Google Patents
A kind of synthetic method of plasma photocatalysis agent and application Download PDFInfo
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- CN107626305A CN107626305A CN201710941876.XA CN201710941876A CN107626305A CN 107626305 A CN107626305 A CN 107626305A CN 201710941876 A CN201710941876 A CN 201710941876A CN 107626305 A CN107626305 A CN 107626305A
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Abstract
A kind of synthetic method of plasma photocatalysis agent includes：By glacial acetic acid, deionized water and ionic liquid [Bmim] [BF4] mixed with butyl titanate under stirring, until after becoming clear state, it is transferred to microwave reaction in 70 milliliters of Teflon liner hydrothermal reaction kettles；Reaction under illumination is blended in metal front liquid solution obtain plasma photocatalysis agent after scrubbed drying.Above-mentioned photochemical catalyst is used for selective oxidation aromatic alcohol compound, by above-mentioned contaminant degradation is aromatic aldehyde compound under visible light conditions, the product of high added value is obtained while effectively removing pollutant；In addition equipment needed for the present invention is simple, simple process, and will not cause additional environmental hazard, realizes the higher value application of aromatic alcohol material, has extremely far-reaching social effect and economic value.
Description
Technical field
The present invention relates to environmental technology field, the synthetic method of especially a kind of plasma photocatalysis agent and application.
Background technology
Energy scarcity has become the global problem for threatening sustainable development with environmental pollution.With Chinese society economy
Development, people's living standard increasingly lifted, eco-living environment is destroyed by irrecoverability, non-renewable fossil energy
Source constantly consumes.Therefore, new regenerative resource is developed, the eco-living environment for improving China is the current important hair in China
Exhibition strategy.Researcher has found that conductor photocatalysis material can convert solar energy into electrical energy or chemical energy in succession, be environment and
The solution of energy problem provides a new effective way, and in recent years, application and the exploration of photocatalysis technology become now
One of research focus of academia.
Research finds that conductor photocatalysis material has potential application value in terms of artificial light compositing, makees in visible ray
Organic pollution can be realized under, the oxidation reaction of hydroxylating, hydrocarbon such as aromatic compound, alcohols chemical combination
The oxidation reaction of thing, the epoxidation reaction of alkene, the aromatic compound reduction reaction containing nitro, CO2Reduce methane phase or methanol
Deng reaction, a brand-new approach is opened for the development and exploration and application of novel photocatalysis material.
But during light-catalysed primitive, photo-generate electron-hole is to the compound and diffusion in body phase or table phase
Transition process is the relation vied each other：From the reaction time, the probability of recombination of photo-generate electron-hole pair spreads far above it
The probability of migration, cause the quantum efficiency of conductor photocatalysis material relatively low.Therefore, reduce photo-generated carrier recombination probability, prolong
In the life-span of long photo-generated carrier, turn into and improve one of photocatalytic activity important channel, and how efficiently to guide photo-generated carrier
Shift, reduce its recombination probability, be subject matter urgently to be resolved hurrily in photocatalysis technology application.
On the other hand, the carbonyls such as aldoketones occupies important as important organic intermediate in chemical process
Status, it is widely used in the fields such as perfume, spices, medicine and additive.In recent years, the environmental consciousness of people gradually strengthens,
And gradually abandoned and used traditional oxidant during conventional alcohol selective oxidation, such as bichromate, permanganate, these oxygen
Agent price is high, poisonous, and inorganic salts waste water is difficult to handle, and environment is caused seriously to pollute, and does not meet current " Green Chemistry "
Requirement.
Because the particularly aromatic series organic matter complexity of the organic pollution in environment is various, by the composition for studying pollutant
Structure, according to its chemical feature, such as C-C, C-OH, C-O-C, C=O chemical bond energies, by the energy model for adjusting catalytic reaction
Enclose, develop a kind of wide spectrum, pollutant is carried out efficient degradation by general catalyst, will effectively reduce organic pollution to environment
Pollution, while obtain high value added product.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of synthetic method of plasma photocatalysis agent
And application, by the synthetic method synthesizing efficient photochemical catalyst of independent research, and selective oxidation aromatic alcohol is used it for as virtue
Fragrant aldehyde, improvement and the recycling of pollutant are realized, eliminate environment and healthy hidden danger.
Technical scheme：
A kind of synthetic method of plasma photocatalysis agent comprises the following steps：
（1）By 3.54 mL glacial acetic acids, 0.35 mL deionized waters and 4.372 mL ionic liquids [Bmim] [BF4] mix, structure
Into reaction solution A；
（2）A certain amount of butyl titanate, speed of agitator 150RPM are added dropwise into reaction solution A, until mixed liquor becomes
Clear state；
（3）Above-mentioned clear mixing liquid is transferred in 70 milliliters of Teflon liner hydrothermal reaction kettles, is subsequently placed into microwave
Clear up in instrument（MDS-6, Shanghai Xin Yi Co., Ltds, China）, 200-280 minutes are reacted at 180-220 DEG C；
（4）Precipitation is collected, with deionized water and absolute ethyl alcohol respectively washing 3 times, is placed in 80 DEG C of baking ovens（SX-G16103, Tianjin middle ring
Electric furnace Co., Ltd, China）Interior drying 24 hours, obtain carrier of photocatalyst.
（5）The above-mentioned carrier of photocatalyst of 10 mg is distributed in the heat resistant glass cup equipped with the methanol solutions of 40 mL 10%,
Appropriate metal front liquid is then added, and encapsulation process is carried out after being filled with argon gas；
（6）With 300W high-pressure sodium lamps（PLS-SXE300, Beijing Bo Feilai Science and Technology Ltd.s, China）It is small to irradiate reaction vessel 2
When；
（7）Liquid color to be mixed is changed into after stable color by white filters out sediment, and in deionized water and absolute ethyl alcohol
Middle cleaning three times, is placed in 80 DEG C of drying in oven 12 hours, finally in Muffle furnace by the catalyst of synthesis with 350 DEG C of calcinings 5
Hour, obtain plasma photocatalysis agent.
Described butyl titanate dosage is ionic liquid [Bmim] [BF4]：Butyl titanate=0.1-5 mol%.
It is gold chloride in described metal front liquid, one kind in silver nitrate, chloroplatinic acid, palladium bichloride, and Au or Ag or Pt
Or 2 wt% that Pd load capacity is catalytic amount.
A kind of application of plasma photocatalysis agent comprises the following steps：
（1）The aromatic alcohol compounds of the above-mentioned photochemical catalysts of 10 mg and 0.1 mmol are added to 1.5 mL benzotrifluoride solvent
In, after being continually fed into the oxygen 5min that purity is 99.99%, sealed reaction vessel；
（2）With 300W xenon sources（PLS-SXE300, Beijing Bo Feilai Science and Technology Ltd.s, China）Irradiate above-mentioned sealing reaction
Container；
（3）Sealed reaction vessel is placed in reaction system（Labsolar-IIIAG, Beijing Bo Feilai Science and Technology Ltd.s, China）In
And the continuous contact of catalyst and reactant is maintained using the magnetic agitation mode in system, its rotating speed is 150RPM, using following
Ring water system carries out temperature control to it, and temperature is 20-30 DEG C；
（4）After reaction terminates, place reaction liquid into 10000RPM centrifuge and centrifuge 5 min, get rid of catalyst, obtain high
The aromatic aldehyde solution of concentration.
Described aromatic alcohol compounds are the organic compound containing phenyl ring and hydroxyl structure.
The advantages of the present invention are：
1. the present invention uses the catalyst of the high visible-light activity with plasma effect, the selectivity of aromatic alcohol is used it for
In oxidation, the catalyst can effectively utilize visible ray, the drawbacks of effectively avoiding existing photocatalysis from playing a role under ultraviolet light,
Improve photocatalysis efficiency；Because the plasma effect of catalyst makes its photoelectric efficiency higher, and the tune of photocatalysis energy
Control so that catalytic selectivity of the invention is up to 99%.
2. equipment is simple needed for the present invention, simple process, and will not cause additional environmental hazard, aromatic alcohol is realized
The degraded of organic pollution, and aromatic aldehyde compound is converted into, the elimination of pollutant is realized, while obtain high added value
Aldehyde product, wherein, the high conversion rate of aromatic alcohol material is up to having extremely far-reaching social effect and economic value.
Embodiment
The present invention is described in further detail by following examples, but the technology contents that are described of the present embodiment be it is illustrative,
Rather than it is limited, protection scope of the present invention should not be limited to according to this.
Embodiment 1：
A kind of synthetic method of plasma photocatalysis agent comprises the following steps：
（1）By 3.54 mL glacial acetic acids, 0.35 mL deionized waters and 4.372 mL ionic liquids [Bmim] [BF4] mix, structure
Into reaction solution A；
（2）Butyl titanate, speed of agitator 150RPM are added dropwise into reaction solution A, until mixed liquor becomes clear
State, wherein ionic liquid [Bmim] [BF4]：The mol% of butyl titanate=0.1；
（3）Above-mentioned clear mixing liquid is transferred in 70 milliliters of Teflon liner hydrothermal reaction kettles, is subsequently placed into microwave
Clear up in instrument, reacted 200 minutes at 180 DEG C；
（4）Precipitation is collected, with deionized water and absolute ethyl alcohol respectively washing 3 times, is placed in 80 DEG C of baking ovens and dries 24 hours, obtain light
Catalyst carrier；
（5）The above-mentioned carrier of photocatalyst of 10 mg is distributed in the heat resistant glass cup equipped with the methanol solutions of 40 mL 10%, then
Chloroplatinic acid precursor liquid is added, and Pt load capacity is 2 wt% of catalytic amount, and carry out encapsulation process after being filled with argon gas；
（6）With 300W high voltage mercury lamp radiations reaction vessel 2 hours；
（7）Liquid color to be mixed is changed into after stable color by white filters out sediment, and in deionized water and absolute ethyl alcohol
Middle cleaning three times, is placed in 80 DEG C of drying in oven 12 hours, finally in Muffle furnace by the catalyst of synthesis with 350 DEG C of calcinings 5
Hour, obtain Pt/TiO2Plasma photocatalysis agent.
A kind of application of plasma photocatalysis agent comprises the following steps：
（1）By the above-mentioned Pt/TiO of 10 mg2Plasma photocatalysis agent and 0.1 mmol phenmethylol compound are added to 1.5 mL
Benzotrifluoride solvent in, be continually fed into purity be 99.99% oxygen 5min after, sealed reaction vessel；
（2）Above-mentioned sealed reaction vessel is irradiated with 300W xenon sources；
（3）Sealed reaction vessel is placed in reaction system and maintains catalyst and reactant using the magnetic agitation mode in system
Continuous contact, its rotating speed is 150RPM, and temperature control is carried out to it using circulation, and temperature is 20 DEG C；
（4）After reaction terminates, place reaction liquid into 10000RPM centrifuge and centrifuge 5 min, get rid of catalyst, obtain high
The benzaldehyde solution of concentration.
Through gas-chromatography and GC-MS analysis shows, the yield of benzaldehyde is up to 99%, and the selectivity of photochemical catalyst is high
Up to more than 99%.
Embodiment 2：
A kind of synthetic method of plasma photocatalysis agent comprises the following steps：
（1）By 3.54 mL glacial acetic acids, 0.35 mL deionized waters and 4.372 mL ionic liquids [Bmim] [BF4] mix, structure
Into reaction solution A；
（2）Butyl titanate, speed of agitator 150RPM are added dropwise into reaction solution A, until mixed liquor becomes clear
State, wherein ionic liquid [Bmim] [BF4]：The mol% of butyl titanate=1；
（3）Above-mentioned clear mixing liquid is transferred in 70 milliliters of Teflon liner hydrothermal reaction kettles, is subsequently placed into microwave
Clear up in instrument, reacted 240 minutes at 200 DEG C；
（4）Precipitation is collected, with deionized water and absolute ethyl alcohol respectively washing 3 times, is placed in 80 DEG C of baking ovens and dries 24 hours, obtain light
Catalyst carrier；
（5）The above-mentioned carrier of photocatalyst of 10 mg is distributed in the heat resistant glass cup equipped with the methanol solutions of 40 mL 10%, then
Chloroplatinic acid precursor liquid is added, Pt load capacity is 2 wt% of catalytic amount, and carries out encapsulation process after being filled with argon gas；
（6）With 300W high voltage mercury lamp radiations reaction vessel 2 hours；
（7）Liquid color to be mixed is changed into after stable color by white filters out sediment, and in deionized water and absolute ethyl alcohol
Middle cleaning three times, is placed in 80 DEG C of drying in oven 12 hours, finally in Muffle furnace by the catalyst of synthesis with 350 DEG C of calcinings 5
Hour, obtain Pt/TiO2Gas ions photochemical catalyst.
A kind of application of plasma photocatalysis agent comprises the following steps：
（1）By the above-mentioned Pt/TiO of 10 mg2Gas ions photochemical catalyst is added to 0.1 mmol's to methylbenzyl alcohol compound
In 1.5 mL benzotrifluoride solvent, after being continually fed into the oxygen 5min that purity is 99.99%, sealed reaction vessel；
（2）Above-mentioned sealed reaction vessel is irradiated with 300W xenon sources；
（3）Sealed reaction vessel is placed in reaction system and maintains catalyst and reactant using the magnetic agitation mode in system
Continuous contact, its rotating speed is 150RPM, and temperature control is carried out to it using circulation, and temperature is 30 DEG C；
（4）After reaction terminates, place reaction liquid into 10000RPM centrifuge and centrifuge 5 min, get rid of catalyst, obtain high
The p-tolyl aldehyde solution of concentration.
Through gas-chromatography and GC-MS analysis shows, the yield of p-tolyl aldehyde is up to more than 99%, photochemical catalyst
Selectivity be up to more than 99%.
Embodiment 3：
A kind of synthetic method of plasma photocatalysis agent comprises the following steps：
（1）By 3.54 mL glacial acetic acids, 0.35 mL deionized waters and 4.372 mL ionic liquids [Bmim] [BF4] mix, structure
Into reaction solution A；
（2）Butyl titanate, speed of agitator 150RPM are added dropwise into reaction solution A, until mixed liquor becomes clear
State, wherein ionic liquid [Bmim] [BF4]：The mol% of butyl titanate=3；
（3）Above-mentioned clear mixing liquid is transferred in 70 milliliters of Teflon liner hydrothermal reaction kettles, is subsequently placed into microwave
Clear up in instrument, reacted 280 minutes at 220 DEG C；
（4）Precipitation is collected, with deionized water and absolute ethyl alcohol respectively washing 3 times, is placed in 80 DEG C of baking ovens and dries 24 hours, obtain light
Catalyst carrier；
（5）The above-mentioned carrier of photocatalyst of 10 mg is distributed in the heat resistant glass cup equipped with the methanol solutions of 40 mL 10%, then
Chloroplatinic acid precursor liquid is added, Pt load capacity is 2 wt% of catalytic amount, and carries out encapsulation process after being filled with argon gas；
（6）With 300W high voltage mercury lamp radiations reaction vessel 2 hours；
（7）Liquid color to be mixed is changed into after stable color by white filters out sediment, and in deionized water and absolute ethyl alcohol
Middle cleaning three times, is placed in 80 DEG C of drying in oven 12 hours, finally in Muffle furnace by the catalyst of synthesis with 350 DEG C of calcinings 5
Hour, obtain plasma photocatalysis agent.
A kind of application of plasma photocatalysis agent comprises the following steps：
（1）The P-methoxybenzyl alcohol compound of the above-mentioned photochemical catalysts of 10 mg and 0.1 mmol is added to 1.5 mL trifluoro
In toluene solvant, after being continually fed into the oxygen 5min that purity is 99.99%, sealed reaction vessel；
（2）Above-mentioned sealed reaction vessel is irradiated with 300W xenon sources；
（3）Sealed reaction vessel is placed in reaction system and maintains catalyst and reactant using the magnetic agitation mode in system
Continuous contact, its rotating speed is 150RPM, and temperature control is carried out to it using circulation, and temperature is 25 DEG C；
（4）After reaction terminates, place reaction liquid into 10000RPM centrifuge and centrifuge 5 min, get rid of catalyst, obtain high
The P-methoxybenzal-dehyde solution of concentration.
Yield through gas-chromatography and GC-MS analysis shows P-methoxybenzal-dehyde is up to more than 99%, photocatalysis
The selectivity of agent is up to more than 99%.
Claims (5)
1. a kind of synthetic method of plasma photocatalysis agent comprises the following steps：
1）By 3.54 mL glacial acetic acids, 0.35 mL deionized waters and 4.372 mL ionic liquids [Bmim] [BF4] mix, form
Reaction solution A；
2）A certain amount of butyl titanate, speed of agitator 150RPM are added dropwise into reaction solution A, until mixed liquor becomes clear
Clear pellucidity；
3）Above-mentioned clear mixing liquid is transferred in 70 milliliters of Teflon liner hydrothermal reaction kettles, microwave is subsequently placed into and disappears
Xie Yizhong, 200-280 minutes are reacted at 180-220 DEG C；
4）Precipitation is collected, with deionized water and absolute ethyl alcohol respectively washing 3 times, is placed in 80 DEG C of baking ovens and dries 24 hours, obtain light
Catalyst carrier；
5）The above-mentioned carrier of photocatalyst of 10 mg is distributed in the heat resistant glass cup equipped with the methanol solutions of 40 mL 10%, then added
Add appropriate metal front liquid, and encapsulation process is carried out after being filled with argon gas；
6）With 300W high voltage mercury lamp radiations reaction vessel 2 hours；
7）Liquid color to be mixed is changed into after stable color by white filters out sediment, and in deionized water and absolute ethyl alcohol
Cleaning three times, is placed in 80 DEG C of drying in oven 12 hours, finally in Muffle furnace that the catalyst of synthesis is small with 350 DEG C of calcinings 5
When, obtain plasma photocatalysis agent.
2. a kind of application of plasma photocatalysis agent comprises the following steps：
1）The aromatic alcohol compounds of the above-mentioned photochemical catalysts of 10 mg and 0.1 mmol are added to 1.5 mL benzotrifluoride solvent
In, after being continually fed into the oxygen 5min that purity is 99.99%, sealed reaction vessel；
2）Above-mentioned sealed reaction vessel is irradiated with 300W xenon sources；
3）Sealed reaction vessel is placed in reaction system and maintains catalyst and reactant using the magnetic agitation mode in system
Continuous contact, its rotating speed is 150RPM, and temperature control is carried out to it using circulation, and temperature is 20-30 DEG C；
4）After reaction terminates, place reaction liquid into 10000RPM centrifuge and centrifuge 5 min, get rid of catalyst, obtain high
The aromatic aldehyde solution of concentration.
3. a kind of synthetic method of plasma photocatalysis agent according to claim 1, it is characterized in that：Described metatitanic acid four
Butyl ester dosage is ionic liquid [Bmim] [BF4]：Butyl titanate=0.1-5 mol%.
4. a kind of synthetic method of plasma photocatalysis agent according to claim 1, it is characterized in that：Before described metal
It is one kind in gold chloride, silver nitrate, chloroplatinic acid, palladium bichloride in drive liquid, and Au or Ag or Pt or Pd load capacity is catalyst
2 wt% of amount.
5. a kind of application of plasma photocatalysis agent according to claim 2, it is characterized in that：Described fragrant alcohol compound
Thing is the organic compound containing phenyl ring and hydroxyl structure.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114011409A (en) * | 2021-12-07 | 2022-02-08 | 南开大学 | Copper monatomic catalyst, preparation method and application thereof, and method for catalytically degrading tetracycline in wastewater by using copper monatomic catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114011409A (en) * | 2021-12-07 | 2022-02-08 | 南开大学 | Copper monatomic catalyst, preparation method and application thereof, and method for catalytically degrading tetracycline in wastewater by using copper monatomic catalyst |
| CN114011409B (en) * | 2021-12-07 | 2022-09-16 | 南开大学 | Copper monatomic catalyst, preparation method and application thereof, and method for catalytically degrading tetracycline in wastewater by using copper monatomic catalyst |
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Application publication date: 20180126 |