CN109908899A - A kind of TiO2Load the preparation method and applications of monatomic Co catalyst - Google Patents
A kind of TiO2Load the preparation method and applications of monatomic Co catalyst Download PDFInfo
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- CN109908899A CN109908899A CN201910194897.9A CN201910194897A CN109908899A CN 109908899 A CN109908899 A CN 109908899A CN 201910194897 A CN201910194897 A CN 201910194897A CN 109908899 A CN109908899 A CN 109908899A
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Abstract
The invention discloses a kind of TiO2The preparation method and applications for loading monatomic Co catalyst belong to novel solid fenton catalyst technical field.Technical solution of the present invention main points are as follows: Co-TiO prepared by the present invention2Catalyst and PMS can activate PMS when acting on and generate SO4 ‑, and be electronically generated hydroxyl radical free radical in hydrone, and then generate high oxidation susceptibility, can be used for handling persistent organic pollutants such as aliphatic organic matter, detergent, dyestuff, pesticide, herbicide, humus etc..The present invention has the characteristics that process flow is simple, environment friendly, at low cost, material have reusing, and the catalytic performance showed in the experiments such as degradation bisphenol-A, dyestuff is excellent.
Description
Technical field
The invention belongs to novel solid fenton catalyst technical fields, and in particular to a kind of TiO2Load monatomic Co catalysis
The preparation method and applications of agent.
Background technique
High-level oxidation technology is the process that pollutant difficult to degrade is removed using the free radical for generating strong oxidizing property.Based on hydroxyl
The Fenton system of base (OH), uses hydrogen peroxide (H2O2) it is used as oxidant, efficiently can almost degrade all organic dirts
Contaminate object.But due to H in Fenton system2O2Poor efficiency and narrow pH sphere of action, greatly limit its practical application.
Class Fenton system generates active oxygen radical as a kind of effective method of cleaning to eliminate present in environment
Persistence organic pollutant.Due to quickly civilising and process of industrialization for human society, class Fenton system is considered as answering
One kind rare to ever-increasing environmental pollution and freshwater resources strategy most with prospects.However, exploitation has enough
The improvement catalyst of activity and stability is still the long term object of practical application.
In recent years, potentiometric titrations (SO is generated by activation permonosulphuric acid salt (PMS)4 -) class Fenton system,
Because of potentiometric titrations (SO4 -) still there is strong oxidizing property within the scope of wide pH, in terms of handling persistence organic pollutant
Obtain extensive concern.The class fenton catalyst for having there are many transition metal to activate as PMS, but most of all there is metal
Ion leaches the problem of with low catalytic performance.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of TiO2Load monatomic Co catalyst preparation method and its
Application in terms of organic pollutant wastewater processing, can effectively improve to the treatment effect of organic pollutant wastewater and save at
This.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of TiO2Load monatomic Co catalyst
Preparation method, it is characterised in that detailed process are as follows:
Step S1: 0.1-1.0g Pluronic F-1270,0.5-5g butyl titanate (TBT) and 10-50mg Cobalt Phthalocyanine are weighed
(CoPC) it is added in the mixed solution that 5-20mL deionized water and 1-10mL n,N-Dimethylformamide (DMF) are formed, ultrasound
Stirring 20-60min forms blue mixed solution；
Step S2: being heated to 300-700 DEG C for quartz ampoule, the side that the blue mixed solution that step S1 is obtained passes through ullrasonic spraying
Method is diffused into the quartz ampoule of 80-180cm, collects the catalyst precursor powder of deposition, is washed with n,N-Dimethylformamide solution
Repeatedly to remove remaining Cobalt Phthalocyanine, the catalyst precursor powder after washing is placed in a vacuum drying oven in 50-100 DEG C of drying；
Step S3: by the powder after step S2 drying process in air atmosphere in 300-600 DEG C of calcining 1-4h, then in flowing
500-1000 DEG C of calcining 1-5h is warming up to the heating rate of 1-5 DEG C/min under argon atmosphere, finally obtained target product TiO2
Load monatomic Co catalyst.
Preferably, the TiO2Load the preparation method of monatomic Co catalyst, it is characterised in that specific steps are as follows:
Step S1: weigh 0.5g Pluronic F-1270,1.0g butyl titanate and 35mg Cobalt Phthalocyanine be added to 15mL go from
In the mixed solution that sub- water and 5mL n,N-Dimethylformamide are formed, ultrasonic agitation 30min forms blue mixed solution；
Step S2: being heated to 600 DEG C for quartz ampoule, and the blue mixed solution that step S1 is obtained is expanded by the method for ullrasonic spraying
Be scattered on the quartz ampoule of 125cm, collect the catalyst precursor powder of deposition, with n,N-Dimethylformamide solution wash repeatedly with
Remaining Cobalt Phthalocyanine is removed, the catalyst precursor powder after washing is placed in a vacuum drying oven in 60 DEG C of dryings；
Step S3: the powder after step S2 is dried is in air atmosphere in 400 DEG C of calcining 2h, then the argon gas gas in flowing
800 DEG C of calcining 2h are warming up to the heating rate of 2 DEG C/min under atmosphere, finally obtained target product TiO2Load monatomic Co catalysis
Agent.
TiO of the present invention2Monatomic Co catalyst is loaded using PMS as oxidizer catalytic degradable organic pollutant
Application in waste water, wherein PMS is the permonosulphuric acid salt that PMS is activation, the TiO2Loading monatomic Co catalyst has very
High stability and heat-resisting and resistance to acid and alkali, TiO2It is that can activate PMS generation that monatomic Co catalyst, which is loaded, with PMS effect
SO4 -, and be electronically generated hydroxyl radical free radical in hydrone, and then generate high oxidation susceptibility, be used for efficient degradation waste water
In organic pollutant, repetitive cycling uses after the cleaned recycling of catalyst after degradation treatment.
TiO of the present invention2Monatomic Co catalyst is loaded using PMS as oxidizer catalytic degradable organic pollutant
Application in waste water, it is characterised in that detailed process are as follows: by TiO2Loading monatomic Co catalyst, to be added to rhdamine B useless
In water, the pH to 3-8 and dark reaction 40min of mixed system are adjusted, oxidant PMS is added, is irradiated with xenon lamp, degradation of dye is useless
Water.
Preferably, the TiO2Loading concentration of the monatomic Co catalyst in waste water from dyestuff is 0.1-50g/L, oxidant
Concentration in waste water from dyestuff is 0.1-2.0g/L.
Co-TiO prepared by the present invention2Catalyst and PMS can activate PMS when acting on and generate SO4 -, and with it is electric in hydrone
Son generates hydroxyl radical free radical, and then generates high oxidation susceptibility, and can be used for handling persistent organic pollutants such as aliphatic has
Machine object, detergent, dyestuff, pesticide, herbicide, humus etc..
Compared with prior art the invention has the following advantages:
1, TiO prepared by the present invention2It loads monatomic Co catalyst and overcomes pure TiO2When as catalyst quantum yield, light
The drawbacks of catalytic efficiency is low and smaller scope of application, shows very high photocatalytic activity in light-catalyzed reaction；
2, TiO produced by the present invention2Monatomic Co catalyst is loaded with very high stability and heat-resisting and resistance to acid and alkali；
3, TiO produced by the present invention2It loads monatomic Co catalyst and still maintains higher catalysis after being recycled for multiple times
Activity has many advantages, such as to be easily recycled and can be recycled.
Detailed description of the invention
Fig. 1 is that TiO is made in embodiment 12Load the TEM figure of monatomic Co catalyst；
Fig. 2 is that TiO is made in embodiment 12Load the SEM figure of monatomic Co catalyst；
Fig. 3 is that TiO is made in embodiment 12Load monatomic Co catalyst, TiO2And the XRD diagram of Co；
Fig. 4 is that TiO is made in embodiment 12Load the EDX mappings image of monatomic Co catalyst；
Fig. 5 is that TiO is made in embodiment 12Monatomic Co catalyst is loaded to the degradation figure of organic pollutant.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
Step S1: weigh 0.5g Pluronic F-1270,1.0g butyl titanate and 35mg Cobalt Phthalocyanine be added to 15mL go from
In the mixed solution that sub- water and 5mL n,N-Dimethylformamide are formed, ultrasonic agitation 30min forms blue mixed solution；
Step S2: being heated to 600 DEG C for quartz ampoule, and the blue mixed solution that step S1 is obtained is expanded by the method for ullrasonic spraying
Be scattered on the quartz ampoule of 125cm, collect the catalyst precursor powder of deposition, with n,N-Dimethylformamide solution wash repeatedly with
Remaining Cobalt Phthalocyanine is removed, the catalyst precursor powder after washing is placed in a vacuum drying oven in 60 DEG C of dryings；
Step S3: the powder after step S2 is dried is in air atmosphere in 400 DEG C of calcining 2h, then the argon gas gas in flowing
800 DEG C of calcining 2h are warming up to the heating rate of 2 DEG C/min under atmosphere, finally obtained target product TiO2Load monatomic Co catalysis
Agent (Co-TiO2).
Embodiment 2
It applies step S1: weighing 0.5g Pluronic F-1270,1.0g butyl titanate and 10mg Cobalt Phthalocyanine and be added to 15mL
In the mixed solution that ionized water and 5mL n,N-Dimethylformamide are formed, ultrasonic agitation 30min forms blue mixed solution；
Step S2: being heated to 600 DEG C for quartz ampoule, and the blue mixed solution that step S1 is obtained is expanded by the method for ullrasonic spraying
Be scattered on the quartz ampoule of 125cm, collect the catalyst precursor powder of deposition, with n,N-Dimethylformamide solution wash repeatedly with
Remaining Cobalt Phthalocyanine is removed, the catalyst precursor powder after washing is placed in a vacuum drying oven in 60 DEG C of dryings；
Step S3: the powder after step S2 is dried is in air atmosphere in 400 DEG C of calcining 2h, then the argon gas gas in flowing
800 DEG C of calcining 2h are warming up to the heating rate of 2 DEG C/min under atmosphere, finally obtained target product TiO2Load monatomic Co catalysis
Agent.
Embodiment 3
Step S1: weigh 0.5g Pluronic F-1270,1.0g butyl titanate and 50mg Cobalt Phthalocyanine be added to 15mL go from
In the mixed solution that sub- water and 5mL n,N-Dimethylformamide are formed, ultrasonic agitation 30min forms blue mixed solution；
Step S2: being heated to 600 DEG C for quartz ampoule, and the blue mixed solution that step S1 is obtained is expanded by the method for ullrasonic spraying
Be scattered on the quartz ampoule of 125cm, collect the catalyst precursor powder of deposition, with n,N-Dimethylformamide solution wash repeatedly with
Remaining Cobalt Phthalocyanine is removed, the catalyst precursor powder after washing is placed in a vacuum drying oven in 60 DEG C of dryings；
Step S3: the powder after step S2 is dried is in air atmosphere in 400 DEG C of calcining 2h, then the argon gas gas in flowing
800 DEG C of calcining 2h are warming up to the heating rate of 2 DEG C/min under atmosphere, finally obtained target product TiO2Load monatomic Co catalysis
Agent.
Embodiment 4
By TiO made from 3mg embodiment 12It loads monatomic Co catalyst and is added in 24mL deionized water simultaneously ultrasonic disperse
6mL rhdamine B waste water is added after the completion, stirs on magnetic stirring apparatus and the pH for adjusting mixed solution is for 20min, ultrasound
9mg oxidant PMS is added in 8, dark reaction 40min；Take 6 1mL centrifuge tubes, number 0,2,4,6,8,10, the centrifuge tube of number 0
It is separately added into methanol solution 0.4mL in middle addition deionized water 0.4mL, 2-10 pipe, for use；It is sampled after dark reaction
0.4mL is added in the centrifuge tube of number 0, and oxidant PMS is added into beaker, opens the light, and timing takes a sample in every two minutes, point
It Jia Ru not be in the centrifuge tube of number 2,4,6,8,10；The absorbance that each sample is surveyed with ultraviolet specrophotometer, calculates sample
Rhodamine B concentration, mapping.
Embodiment 5
By 3mg TiO2It is added in 24mL deionized water and 6mL rhodamine B dye is added in ultrasonic disperse 20min, ultrasound after the completion
Expect waste water, the pH that mixed solution is stirred and adjusted on magnetic stirring apparatus is 8, dark reaction 40min, and 9mg oxidant PMS is added；
Take 6 1mL centrifuge tubes, deionized water 0.4mL, 2-10 Guan Zhongfen is added in the centrifuge tube of number 0 in number 0,2,4,6,8,10
Not Jia Ru methanol solution 0.4mL, for use；0.4mL is sampled after dark reaction to be added in the centrifuge tube of number 0, is added into beaker
Enter oxidant PMS, open the light, timing takes a sample in every two minutes, is separately added into the centrifuge tube of number 2,4,6,8,10；With purple
The absorbance of outer spectrophotometric measurement each sample, calculates the rhodamine B concentration of sample, maps.
Embodiment 6
It takes 24mL deionized water to be added in beaker, adds 6mL rhdamine B waste water, stirred simultaneously on magnetic stirring apparatus
The pH for adjusting mixed solution is 8, dark reaction 40min, and 9mg oxidant PMS is added；Take 6 1mL centrifuge tubes, number 0,2,4,6,
8,10, deionized water 0.4mL is added in the centrifuge tube of number 0, is separately added into methanol solution 0.4mL in 2-10 pipe, for use；Secretly
Sampling 0.4mL is added in the centrifuge tube of number 0 after reaction, and oxidant PMS is added into beaker, opens the light, timing, and every two points
Clock takes a sample, is separately added into the centrifuge tube of number 2,4,6,8,10；The absorbance of each sample is surveyed with ultraviolet specrophotometer,
The rhodamine B concentration of sample is calculated, is mapped.
Embodiment 7
By TiO made from 3mg embodiment 12It loads monatomic Co catalyst and is added in 24mL deionized water simultaneously ultrasonic disperse
6mL rhdamine B waste water is added after the completion, stirs on magnetic stirring apparatus and the pH for adjusting mixed solution is for 20min, ultrasound
8, dark reaction 40min；Take 6 1mL centrifuge tubes, deionized water is added in the centrifuge tube of number 0 in number 0,2,4,6,8,10
Methanol solution 0.4mL is separately added into 0.4mL, 2-10 pipe, for use；After dark reaction sample 0.4mL be added number 0 from
It in heart pipe, opens the light, timing takes a sample in every two minutes, is separately added into the centrifuge tube of number 2,4,6,8,10；Use ultraviolet spectrometry
Luminosity measures the absorbance of each sample, calculates the rhodamine B concentration of sample, maps.
Embodiment 8
By TiO made from 3mg embodiment 12It loads monatomic Co catalyst and is added in 24mL deionized water simultaneously ultrasonic disperse
6mL rhdamine B waste water is added after the completion, stirs on magnetic stirring apparatus and the pH for adjusting mixed solution is for 20min, ultrasound
9mg oxidant PMS is added in 8, dark reaction 40min；Take 6 1mL centrifuge tubes, number 0,2,4,6,8,10, the centrifuge tube of number 0
It is separately added into methanol solution 0.4mL in middle addition deionized water 0.4mL, 2-10 pipe, for use；It is sampled after dark reaction
0.4mL is added in the centrifuge tube of number 0, and oxidant PMS is added into beaker, and timing takes a sample in every two minutes, is separately added into
In the centrifuge tube of number 2,4,6,8,10；The absorbance that each sample is surveyed with ultraviolet specrophotometer, calculates the rhodamine B of sample
Concentration, mapping.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (5)
1. a kind of TiO2Load the preparation method of monatomic Co catalyst, it is characterised in that detailed process are as follows:
Step S1: 0.1-1.0g Pluronic F-1270,0.5-5g butyl titanate and 10-50mg Cobalt Phthalocyanine are weighed and is added to
In the mixed solution that 5-20mL deionized water and 1-10mL n,N-Dimethylformamide are formed, ultrasonic agitation 20-60min is formed
Blue mixed solution；
Step S2: being heated to 300-700 DEG C for quartz ampoule, the side that the blue mixed solution that step S1 is obtained passes through ullrasonic spraying
Method is diffused into quartz ampoule, on the quartz ampoule of 80-180cm, collects the catalyst precursor powder of deposition, with N, N- dimethyl formyl
Amine aqueous solution washs repeatedly to remove remaining Cobalt Phthalocyanine, and the catalyst precursor powder after washing is placed in a vacuum drying oven in 50-
100 DEG C of dryings；
Step S3: by the powder after step S2 drying process in air atmosphere in 300-600 DEG C of calcining 1-4h, then in flowing
500-1000 DEG C of calcining 1-5h is warming up to the heating rate of 1-5 DEG C/min under argon atmosphere, finally obtained target product TiO2
Load monatomic Co catalyst.
2. TiO according to claim 12Load the preparation method of monatomic Co catalyst, it is characterised in that specific steps
Are as follows:
Step S1: weigh 0.5g Pluronic F-1270,1.0g butyl titanate and 35mg Cobalt Phthalocyanine be added to 15mL go from
In the mixed solution that sub- water and 5mL n,N-Dimethylformamide are formed, ultrasonic agitation 30min forms blue mixed solution；
Step S2: 600 DEG C are heated to by vacuum pump, the blue mixed solution that the method for ullrasonic spraying obtains step S1 is spread
Onto the quartz ampoule of 125cm, the catalyst precursor powder of deposition is collected, is washed repeatedly with n,N-Dimethylformamide solution to go
Except remaining Cobalt Phthalocyanine, the catalyst precursor powder after washing is placed in a vacuum drying oven in 60 DEG C of dryings；
Step S3: the powder after step S2 is dried is in air atmosphere in 400 DEG C of calcining 2h, then the argon gas gas in flowing
800 DEG C of calcining 2h are warming up to the heating rate of 2 DEG C/min under atmosphere, finally obtained target product TiO2Load monatomic Co catalysis
Agent.
3. TiO made from method according to claim 1 or 22Monatomic Co catalyst is loaded using PMS as oxidant
Application in catalytic degradation organic pollutant wastewater, wherein PMS is the permonosulphuric acid salt that PMS is activation, the TiO2Load is single
Atom Co catalyst has very high stability and heat-resisting and resistance to acid and alkali, TiO2It loads monatomic Co catalyst and PMS is acted on
It is that can activate PMS to generate SO4 -, and be electronically generated hydroxyl radical free radical in hydrone, and then generate high oxidation susceptibility,
For the organic pollutant in efficient degradation waste water, repetitive cycling is used after the cleaned recycling of catalyst after degradation treatment.
4. application according to claim 3, it is characterised in that detailed process are as follows: by TiO2Monatomic Co catalyst is loaded to add
Enter into rhdamine B waste water, adjusts the pH to 3-8 and dark reaction 40min of mixed system, oxidant PMS is added, uses xenon lamp
Irradiation, degradation of dye waste water.
5. application according to claim 4, it is characterised in that: the TiO2Monatomic Co catalyst is loaded in waste water from dyestuff
In concentration be 0.1-50g/L, concentration of the oxidant in waste water from dyestuff be 0.1-2.0g/L.
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| CN110227458A (en) * | 2019-07-22 | 2019-09-13 | 四川轻化工大学 | A kind of composite material of Copper-cladding Aluminum Bar mesoporous TiO 2 and its application |
| CN112023690A (en) * | 2020-08-26 | 2020-12-04 | 福建龙净环保股份有限公司 | VOCs waste gas treatment system and VOCs waste gas treatment method |
| WO2021031056A1 (en) * | 2019-08-19 | 2021-02-25 | 中山大学 | Method for preparing monatomic catalyst by means of atomization of precursor |
| CN113617344A (en) * | 2021-07-29 | 2021-11-09 | 联科华技术有限公司 | Monoatomic photocatalytic plate for sewage treatment and preparation method thereof |
| CN116159560A (en) * | 2023-04-24 | 2023-05-26 | 上海交通大学内蒙古研究院 | Composite photocatalyst and preparation method and application thereof |
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| CN113617344B (en) * | 2021-07-29 | 2023-09-26 | 联科华技术有限公司 | Monoatomic photocatalytic plate for sewage treatment and preparation method thereof |
| CN116159560A (en) * | 2023-04-24 | 2023-05-26 | 上海交通大学内蒙古研究院 | Composite photocatalyst and preparation method and application thereof |
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