CN107626339A - A kind of synthetic method of the selective oxidation photochemical catalyst of molecular sieve carrier and application - Google Patents
A kind of synthetic method of the selective oxidation photochemical catalyst of molecular sieve carrier and application Download PDFInfo
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Abstract
A kind of synthetic method of the selective oxidation photochemical catalyst of molecular sieve carrier includes：Molecular sieve carrier is disperseed in absolute ethyl alcohol and butyl titanate, the microwave reaction in Teflon liner hydrothermal reaction kettle is added dropwise；Quickly heating chlorauric acid solution and Au/TiO using molecular sieve as carrier is obtained after micro-wave digestion scrubbed drying in 5 minutes under ar gas environment after reaction2/ molecular sieve visible light catalyst.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 synthesis of the selective oxidation photochemical catalyst of especially a kind of molecular sieve carrier
Method 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 selective oxidation light of molecular sieve carrier to urge
The synthetic method of agent and application, by the synthetic method synthesizing efficient photochemical catalyst of independent research, and use it for selectivity
Oxidation aromatic alcohol is aromatic aldehyde, realizes improvement and the recycling of pollutant, eliminates environment and healthy hidden danger.
Technical scheme：
A kind of synthetic method of the selective oxidation photochemical catalyst of molecular sieve carrier comprises the following steps：
（1）1g molecular sieve carrier is added to ultrasonic disperse two hours in 10-30 mL absolute ethyl alcohol, obtains absolute ethyl alcohol point
Dispersion liquid；
（2）It is added dropwise 1-4g butyl titanate into absolute ethyl alcohol dispersion liquid, at the same magnetic agitation 1 hour, speed of agitator
150RPM；
（3）Above-mentioned mixing liquid is transferred in 70 milliliters of Teflon liner hydrothermal reaction kettles, is subsequently placed into microwave dissolver
（MDS-6, Shanghai Hai Xin instrument Co., Ltd, China）, 20-40 minutes are reacted at 150-200 DEG C；
（4）Precipitation is collected, with 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 have
Limit company, China）Interior drying 24 hours；
（5）The interior baking of baking oven for taking the above-mentioned dried powders of 0.5-1g to be placed in 120 DEG C 1 hour；
（6）By a certain amount of chlorauric acid solution（10 mg/mL）Rapidly join, and 1-5min is maintained under negative pressure system；
（7）Under ar gas environment, microwave reaction 5 minutes in microwave dissolver；
（8）Above-mentioned reaction precipitation is washed 3 times respectively with distilled water and absolute ethyl alcohol, is then dried 24 hours in 80 DEG C of baking ovens,
The Au/TiO using molecular sieve as carrier can be obtained2/ molecular sieve visible light catalyst.
Described molecular sieve catalyst includes SBA-15, X-type, Y types, modenite, ZSM-5.
Described chlorauric acid solution dosage is Au：Catalyst=0.5-2 wt%.
A kind of application of the selective oxidation photochemical catalyst of molecular sieve carrier comprises the following steps：
（1）The aromatic alcohol compounds of the above-mentioned photochemical catalysts of 10 mg and 0.1 mmol are added in 5 mL toluene solvant, are filled with
Purity is 99.99% min of oxygen 5, and with polytetrafluorethylescrewed screwed seal cap sealed reaction vessel；
（2）With 300W xenon sources（PLS-SXE300, Beijing Bo Feilai Science and Technology Ltd.s, China）Irradiate reaction vessel；
（3）Reaction vessel is placed in reaction system（Labsolar-IIIAG, Beijing Bo Feilai Science and Technology Ltd.s, China）In and adopt
The continuous contact of catalyst and reactant is maintained with the magnetic agitation mode in system, its rotating speed is 150RPM, utilizes recirculated water
System carries out temperature control to it, and temperature is 20-30 DEG C；
（4）After reaction terminates, 10000RPM centrifuge is placed reaction liquid into（TG16-WS, the limited public affairs of Hunan Hunan instrument centrifuge
Department, China）5 min of middle centrifugation, get rid of catalyst, obtain the aromatic aldehyde solution of high 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 molecular sieve as the active component of carrier appendix visible light catalytic, the selective oxygen of aromatic alcohol is used it for
In change, the catalyst can effectively utilize visible ray, the drawbacks of effectively avoiding existing photocatalysis from playing a role under ultraviolet light, carry
High photocatalysis efficiency；Due to unique pore passage structure of molecular sieve, and the regulation and control of photocatalysis energy so that catalysis of the invention
Selectivity 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 the selective oxidation photochemical catalyst of molecular sieve carrier comprises the following steps：
（1）1g SBA-15 molecular sieve carriers are added to ultrasonic disperse two hours in 10 mL absolute ethyl alcohol, obtain absolute ethyl alcohol
Dispersion liquid；
（2）It is added dropwise 1g butyl titanate into absolute ethyl alcohol dispersion liquid, at the same magnetic agitation 1 hour, speed of agitator
150RPM；
（3）Above-mentioned mixing liquid is transferred in 70 milliliters of Teflon liner hydrothermal reaction kettles, is subsequently placed into microwave dissolver,
Reacted 20 minutes at 150 DEG C；
（4）Precipitation is collected, with water and absolute ethyl alcohol respectively washing 3 times, is placed in 80 DEG C of baking ovens and dries 24 hours；
（5）The interior baking of baking oven for taking the above-mentioned dried powders of 0.5g to be placed in 120 DEG C 1 hour；
（6）By a certain amount of chlorauric acid solution（10 mg/mL）Rapidly join, and 2min is maintained under negative pressure system, wherein, Au：
Catalyst=0.5wt %；
（7）Under ar gas environment, microwave reaction 5 minutes in microwave dissolver；
（8）Above-mentioned reaction precipitation is washed 3 times respectively with distilled water and absolute ethyl alcohol, is then dried 24 hours in 80 DEG C of baking ovens,
The Au/TiO using molecular sieve as carrier can be obtained2/ SBA-15 visible light catalysts.
A kind of application of the selective oxidation photochemical catalyst of molecular sieve carrier comprises the following steps：
（1）The phenmethylol compound of the above-mentioned photochemical catalysts of 10 mg and 0.1 mmol is added in 5 mL toluene solvant, is filled with
Purity is 99.99% min of oxygen 5, and with polytetrafluorethylescrewed screwed seal cap sealed reaction vessel；
（2）Reaction vessel is irradiated with 300W xenon sources；
（3）Reaction vessel is placed in reaction system and maintains holding for catalyst and reactant using the magnetic agitation mode in system
Continued access is touched, and its rotating speed is 150RPM, temperature control is carried out to it using circulation, temperature is 20 DEG C；
（4）After reaction terminates, extraction 0.5 mL reaction solutions dilution, it is placed in 10000RPM centrifuge and centrifuges 5 min, get rid of
Catalyst, obtain benzaldehyde solution.
Yield through gas-chromatography and GC-MS analysis shows benzaldehyde is up to more than 91%, the selection of photochemical catalyst
Property is up to more than 99%.
Embodiment 2：
A kind of synthetic method of the selective oxidation photochemical catalyst of molecular sieve carrier comprises the following steps：
（1）1g SBA-15 molecular sieve carriers are added to ultrasonic disperse two hours in 20 mL absolute ethyl alcohol, obtain absolute ethyl alcohol
Dispersion liquid；
（2）It is added dropwise 2g butyl titanate into absolute ethyl alcohol dispersion liquid, at the same magnetic agitation 1 hour, speed of agitator
150RPM；
（3）Above-mentioned mixing liquid is transferred in 70 milliliters of Teflon liner hydrothermal reaction kettles, is subsequently placed into microwave dissolver,
Reacted 30 minutes at 180 DEG C；
（4）Precipitation is collected, with water and absolute ethyl alcohol respectively washing 3 times, is placed in 80 DEG C of baking ovens and dries 24 hours；
（5）The interior baking of baking oven for taking the above-mentioned dried powders of 0.5g to be placed in 120 DEG C 1 hour；
（6）By a certain amount of chlorauric acid solution（10 mg/mL）Rapidly join, and 5min, wherein Au are maintained under negative pressure system：
The wt% of catalyst=1；
（7）Under ar gas environment, microwave reaction 5 minutes in microwave dissolver；
（8）Above-mentioned reaction precipitation is washed 3 times respectively with distilled water and absolute ethyl alcohol, is then dried 24 hours in 80 DEG C of baking ovens,
The Au/TiO using molecular sieve as carrier can be obtained2/ SBA-15 visible light catalysts.
A kind of application of the selective oxidation photochemical catalyst of molecular sieve carrier comprises the following steps：
（1）The P-methoxybenzyl alcohol of the above-mentioned photochemical catalysts of 10 mg and 0.1 mmol is added in 5 mL toluene solvant, filled
Enter the min of oxygen 5 that purity is 99.99%, and with polytetrafluorethylescrewed screwed seal cap sealed reaction vessel；
（2）Reaction vessel is irradiated with 300W xenon sources；
（3）Reaction vessel is placed in reaction system and maintains holding for catalyst and reactant using the magnetic agitation mode in system
Continued access is touched, and its rotating speed is 150RPM, temperature control is carried out to it using circulation, 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-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%.
Embodiment 3：
A kind of synthetic method of the selective oxidation photochemical catalyst of molecular sieve carrier comprises the following steps：
（1）1g ZSM-5 molecular sieve carrier is added to ultrasonic disperse two hours in 30 mL absolute ethyl alcohol, obtains absolute ethyl alcohol
Dispersion liquid；
（2）It is added dropwise 4g butyl titanate into absolute ethyl alcohol dispersion liquid, at the same magnetic agitation 1 hour, speed of agitator
150RPM；
（3）Above-mentioned mixing liquid is transferred in 70 milliliters of Teflon liner hydrothermal reaction kettles, is subsequently placed into microwave dissolver,
Reacted 40 minutes at 200 DEG C；
（4）Precipitation is collected, with water and absolute ethyl alcohol respectively washing 3 times, is placed in 80 DEG C of baking ovens and dries 24 hours；
（5）The interior baking of baking oven for taking the above-mentioned dried powders of 1g to be placed in 120 DEG C 1 hour；
（6）By a certain amount of chlorauric acid solution（10 mg/mL）Rapidly join, and 1-5min is maintained under negative pressure system, wherein
Au：The wt% of catalyst=2；
（7）Under ar gas environment, microwave reaction 5 minutes in microwave dissolver；
（8）Above-mentioned reaction precipitation is washed 3 times respectively with distilled water and absolute ethyl alcohol, is then dried 24 hours in 80 DEG C of baking ovens,
The Au/TiO using molecular sieve as carrier can be obtained2/ ZSM-5 visible light catalysts.
A kind of application of the selective oxidation photochemical catalyst of molecular sieve carrier comprises the following steps：
（1）By the above-mentioned photochemical catalysts of 10 mg and the 0.1 mmol toluene solvant that 5 mL are added to methylbenzyl alcohol compound
In, the min of oxygen 5 that purity is 99.99% is filled with, and with polytetrafluorethylescrewed screwed seal cap sealed reaction vessel；
（2）Reaction vessel is irradiated with 300W xenon sources；
（3）Reaction vessel is placed in reaction system and maintains holding for catalyst and reactant using the magnetic agitation mode in system
Continued access is touched, and its rotating speed is 150RPM, temperature control is carried out to it using circulation, 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.
Yield through gas-chromatography and GC-MS analysis shows p-tolyl aldehyde is up to more than 93%, photochemical catalyst
Selectivity be up to more than 99%.
Claims (5)
1. a kind of synthetic method of the selective oxidation photochemical catalyst of molecular sieve carrier comprises the following steps：
1）1g molecular sieve carrier is added to ultrasonic disperse two hours in 10-30 mL absolute ethyl alcohol, absolute ethyl alcohol is obtained and disperses
Liquid；
2）It is added dropwise 1-4g butyl titanate into absolute ethyl alcohol dispersion liquid, at the same magnetic agitation 1 hour, speed of agitator
150RPM；
3）Above-mentioned mixing liquid is transferred in 70 milliliters of Teflon liner hydrothermal reaction kettles, is subsequently placed into microwave dissolver,
20-40 minutes are reacted at 150-200 DEG C；
4）Precipitation is collected, with water and absolute ethyl alcohol respectively washing 3 times, is placed in 80 DEG C of baking ovens and dries 24 hours；
5）The interior baking of baking oven for taking the above-mentioned dried powders of 0.5-1g to be placed in 120 DEG C 1 hour；
6）By a certain amount of chlorauric acid solution（10 mg/mL）Rapidly join, and 1-5min is maintained under negative pressure system；
7）Under ar gas environment, microwave reaction 5 minutes in microwave dissolver；
8）Above-mentioned reaction precipitation is washed 3 times respectively with distilled water and absolute ethyl alcohol, is then dried 24 hours in 80 DEG C of baking ovens, can
Obtain the Au/TiO using molecular sieve as carrier2/ molecular sieve visible light catalyst.
2. a kind of application of the selective oxidation photochemical catalyst of molecular sieve carrier comprises the following steps：
1）The aromatic alcohol compounds of the above-mentioned photochemical catalysts of 10 mg and 0.1 mmol are added in 5 mL toluene solvant, are filled with
Purity is 99.99% min of oxygen 5, and with polytetrafluorethylescrewed screwed seal cap sealed reaction vessel；
2）Reaction vessel is irradiated with 300W xenon sources；
3）Reaction vessel is placed in reaction system and maintains holding for catalyst and reactant using the magnetic agitation mode in system
Continued access is touched, and its rotating speed is 150RPM, temperature control is carried out to it using circulation, 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 the selective oxidation photochemical catalyst of molecular sieve carrier according to claim 1, its feature
For：Described molecular sieve catalyst includes SBA-15, X-type, Y types, modenite, ZSM-5.
4. a kind of synthetic method of the selective oxidation photochemical catalyst of molecular sieve carrier according to claim 1, its feature
For：Described chlorauric acid solution dosage is Au：Catalyst=0.5-2 wt%.
5. a kind of application of the selective oxidation photochemical catalyst of molecular sieve carrier according to claim 2, it is characterized in that：Institute
The aromatic alcohol compounds stated are the organic compound containing phenyl ring and hydroxyl structure.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113198530A (en) * | 2021-05-10 | 2021-08-03 | 江南大学 | Au-Mg/SAPO-11 molecular sieve catalyst, and preparation method and application thereof |
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| CN103599806A (en) * | 2013-12-03 | 2014-02-26 | 福州大学 | Photocatalyst used for synthesis of aromatic aldehyde chemical and preparation method thereof |
| CN103691477A (en) * | 2013-12-27 | 2014-04-02 | 天津城建大学 | Preparation method of binary load-type TiO2/nano-iron/SBA-15 catalyst |
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2017
- 2017-10-11 CN CN201710941875.5A patent/CN107626339A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103599806A (en) * | 2013-12-03 | 2014-02-26 | 福州大学 | Photocatalyst used for synthesis of aromatic aldehyde chemical and preparation method thereof |
| CN103691477A (en) * | 2013-12-27 | 2014-04-02 | 天津城建大学 | Preparation method of binary load-type TiO2/nano-iron/SBA-15 catalyst |
Non-Patent Citations (2)
| Title |
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| CHEN Y等: "Gold nanoparticle-modified TiO2/SBA-15 nanocomposites as active plasmonic photocatalysts for the selective oxidation of aromatic alcohols", 《RSC ADVANCES》 * |
| YU CHEN 等: "Microwave-assistedhydrothermalsynthesisofAu/TiO2/SBA-15", 《MATERIALS LETTERS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113198530A (en) * | 2021-05-10 | 2021-08-03 | 江南大学 | Au-Mg/SAPO-11 molecular sieve catalyst, and preparation method and application thereof |
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Application publication date: 20180126 |