CN107175093A - A kind of method that ordered mesoporous carbon composite material of boron atom modification activates persulfate degradation of organic substances - Google Patents
A kind of method that ordered mesoporous carbon composite material of boron atom modification activates persulfate degradation of organic substances Download PDFInfo
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- CN107175093A CN107175093A CN201710559414.1A CN201710559414A CN107175093A CN 107175093 A CN107175093 A CN 107175093A CN 201710559414 A CN201710559414 A CN 201710559414A CN 107175093 A CN107175093 A CN 107175093A
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- persulfate
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- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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Abstract
The invention belongs to water treatment field, and in particular to a kind of preparation of boron doping ordered mesoporous carbon composite material and its method for activation persulfate degradation of organic substances.The present invention is prepared for nonmetallic boron doping ordered mesopore carbon composite catalyst (B OMC) using the method for evaporation-induced self-assembly, uses it for activating persulfate.Catalyst amountses are 0.1 0.3g/L, and persulfate concentration is 0.5-2.0mM, under room temperature condition, and processing time is 90min, and the method can realize the efficient degradation of Some Organic Pollutants.After testing, singlet oxygen (1O2) free radical plays main oxidation in this process.
Description
Technical field
The invention belongs to water treatment field, and in particular to a kind of preparation and its work of boron doping ordered mesoporous carbon composite material
Change the method for persulfate degradation of organic substances.
Background technology
With the development of the city with the quickening of process of industrialization, water environment pollution especially persistence difficult degradation organic contamination
The harm of thing is increasingly serious.This kind of persistent organic pollutants in water body distribution extensively, the time length that retains, to nature
The harm of environment and the mankind is big, intractability is big, and the research of its treatment technology is always the focus of environmentalist's concern.In recent years
Come, high-level oxidation technology (the Advanced Oxidation with the characteristics of the hydroxyl radical free radical (OH) for producing high reaction activity
Processes abbreviation AOPs) appearance handle pollutant in water body for us and provide new idea and method.Hydroxyl radical free radical
A series of radical chain reactions can be induced, various organic pollutions are attacked to non-selectivity, low toxicity are degraded into or nontoxic
Small-molecule substance, or even directly mineralising be CO2, water, reach the purpose of environmental treatment.
It is excellent because oxidability is strong, selectivity is high, applicable pH range is wide etc. based on the high-level oxidation technology of activation persulfate
Point is of increasing concern.Persulfate can produce the sulfuric acid of strong oxidizing property under the effect such as light, heat, electricity and transition metal ions
Root free radical (SO4 ·-) and OH, efficient degradation organic pollution.Wherein, with the physically activated process energy of light, heat, electricity for representative
Consumption is high, difficult regulation and control.Transition metal ions activates persulfate, because of the input without external energy, it is more economical with it is efficient and obtain
To widely studied, but also it there is the potential danger that digestion of metallic ion causes secondary pollution of water simultaneously.Ordered mesopore carbon
(OMC) as typical non-metallic catalyst, with high specific surface area, homogeneous pore passage structure, the abundant oxygen-containing official in its surface
It can roll into a ball as active site, there is certain activity function to potassium hydrogen persulfate (PMS), but its catalytic activity still needs to be carried
It is high.
The application is prepared for nonmetallic boron doped order mesoporous carbon composite catalytic using the method for evaporation-induced self-assembly
Agent (B-OMC), uses it for activating persulfate, can realize the efficient degradation of organic contamination pollutant.
The content of the invention
Instant invention overcomes physically activated including ultraviolet light, heating, microwave etc., and the method such as transition metal ions activation
The defect of persulfate is activated, by preparing nonmetallic boron doping ordered mesopore carbon composite catalyst, activation persulfate is produced
Living radical, efficient degradation stubbornness organic pollution.
In order to realize the above object the present invention is adopted the following technical scheme that：
100mL organic pollution materials are added in the reactor, 0.1-0.3g/L B-OMC catalyst is added, and adsorb 30min
Reach after saturation, add 0.5-2.0mM PMS, react 60min.
Described nonmetallic boron doping ordered mesopore carbon method for preparing composite catalyst is as follows：
(1) preparation of B-Resol types phenolic resin：Phenol and NaOH are dissolved in the water, and are then slowly added dropwise a certain amount of
37wt.% formalins, are heated to 75 DEG C of reaction 0.5h by this mixture, add H3BO3Continue to react 1h.2M is used after cooling
HCl adjusts pH to neutrality, and then moisture removal is removed in vacuum distillation under the conditions of 45 DEG C, and Resol type novolak resin precursor body weight is newly molten
Solution (mass fraction is 20%) in ethanol, stands filtering after 24h and removes the NaCl crystal separated out.
(2) a certain amount of F127 is dissolved in ethanol, then adds the ethanol solution of 20wt.%B-Resol type phenolic resin,
The solution is transferred in culture dish after stirring 10min, volatilize 4-8h at room temperature, then culture dish is placed in 100 DEG C of baking ovens admittedly
Change 24h, obtain thin-film material.Film is scraped from culture dish with scraper, the polymer composite of ordered structure is obtained, by this
Compound is placed in N in tube furnace2800 DEG C of calcinings, products therefrom grind into powder in atmosphere.
Described organic pollution, including bisphenol-A, phenol, 2,4- Dichlorophenols and radonil etc..
A kind of boron doping ordered mesoporous carbon composite material (B-OMC) of the present invention activates the side of persulfate degradation of organic substances
Method, principle be persulfate be stimulated under B-OMC catalytic action generation singlet oxygen (1O2), its degraded to organic pollution
Play main function.
The features of the present invention is as follows：
1. preparing the Resol resins of boron-doping, make boron dispersed, in stable incorporation OMC carbon skeleton, material has homogeneous
Neat pore passage structure.
2. nonmetallic modifying carbon material activates persulfate, the input of no added metal and heat, light and electricity etc., energy-conservation and ring
Efficiently activation persulfate is realized under conditions of border is friendly.
3. course of reaction produces strong oxidizing property1O2, can Quick Oxidation decomposing organic pollutant.
Brief description of the drawings
1. Fig. 1 is the transmission electron micrograph of the boron doping ordered mesoporous carbon composite material prepared；
2. Fig. 2 is the effect of the different organic pollutions of boron doping ordered mesoporous carbon composite material activation potassium hydrogen persulfate degraded
Figure.
Embodiment：
Embodiment 1
The bisphenol-A solution 100mL that concentration is 20mg/L is added in the reactor, adds 0.1g/L B-OMC-800 catalysis
After agent, absorption 30min, 1mM PMS are added, 60min is reacted, the clearance of bisphenol-A reaches 91%.
Embodiment 2
The phenol solution 100mL that concentration is 20mg/L is added in the reactor, adds 0.1g/L B-OMC-800 catalyst,
Adsorb after 30min, add 1mM PMS, react 60min, the degradation efficiency of phenol is 87%.
Embodiment 3
2, the 4- dichloro phenol solution 100mL that concentration is 20mg/L are added in the reactor, add 0.1g/L B-OMC-800
After catalyst, absorption 30min, 1mM PMS are added, 60min are reacted, the degradation efficiency of 2,4- Dichlorophenols is 99%.
Embodiment 4
The radonil solution 100mL that concentration is 20mg/L is added in the reactor, adds 0.1g/L B-OMC-800 catalysis
After agent, absorption 30min, 1mM PMS are added, 60min are reacted, the degradation efficiency of radonil is 99%.
Claims (5)
1. a kind of method that boron doped ordered mesoporous carbon composite material activates persulfate degradation of organic substances, it is characterised in that
Using block copolymer F127 as template, composite catalyst is prepared by the method for evaporation-induced self-assembly.
2. a kind of boron doped ordered mesoporous carbon composite material as described in right 1 activates the side of persulfate degradation of organic substances
Method, it is characterised in that prepared by the material comprises the following steps：
(1) preparation of B-Resol types phenolic resin：Phenol and NaOH are dissolved in the water, and a certain amount of 37wt.% is then slowly added dropwise
Formalin, is heated to 75 DEG C of reaction 0.5h by this mixture, adds H3BO3Continue to react 1h, be cooled to after room temperature and use 2M HCl
PH is adjusted to neutrality, then moisture removal is removed in vacuum distillation under the conditions of 45 DEG C, and Resol type novolak resin precursor bodies are redissolved in
In ethanol (mass fraction is 20%), stand filtering after 24h and remove the NaCl crystal separated out；
(2) a certain amount of F127 is dissolved in ethanol, then adds the ethanol solution of 20wt.%B-Resol type phenolic resin, stirring
The solution is transferred in culture dish after certain time, volatilized at room temperature complete, then culture dish is placed in progress in 100 DEG C of baking ovens
Solidification, obtains thin-film material, scrapes from culture dish film with scraper, obtains the polymer composite of ordered structure, finally
The compound is placed in N in tube furnace2Calcined in atmosphere under certain temperature, products therefrom grind into powder.
3. a kind of boron doped ordered mesoporous carbon composite material activation persulfate degradation of organic substances as described in right 1 and 2
Method, it is characterised in that comprise the following steps that, catalyst amountses are 0.1-0.3g/L, persulfate concentration is 0.5-
Under 2.0mM, room temperature condition, processing time is 90 minutes.
4. a kind of boron doped ordered mesoporous carbon composite material activation persulfate degradation of organic substances as described in right 1 and 2
Method, it is characterised in that the persulfate added can be potassium peroxydisulfate or sodium peroxydisulfate or ammonium persulfate-sodium bisulfate, is added total
Concentration is 0.2-2.0mM.
5. a kind of boron doped ordered mesoporous carbon composite material activation persulfate degradation of organic substances as described in right 1 and 2
Method, it is characterised in that during by this method four kinds of organic matter (bisphenol-A, phenol, 2,4- Dichlorophenols and radonils) of degraded, drop
Efficiency is solved respectively up to 91%, 87%, 99% and 99%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110302769A (en) * | 2018-03-20 | 2019-10-08 | 中国科学院大连化学物理研究所 | A kind of catalyst carrier, loaded catalyst and its preparation method and application |
| CN110652978A (en) * | 2019-08-27 | 2020-01-07 | 浙江理工大学 | Preparation method and application of nonmetal modified carbon fiber |
| CN111111637A (en) * | 2019-12-31 | 2020-05-08 | 太原理工大学 | Boron-doped non-metallic catalyst and preparation method and application thereof |
| CN111450865A (en) * | 2020-04-28 | 2020-07-28 | 中山大学 | Preparation method and application of catalyst for oxidative degradation of bisphenol A by sulfate radical |
| CN112441659A (en) * | 2019-08-30 | 2021-03-05 | 湖南大学 | Method for degrading and treating organic pollutants by activating persulfate through multi-stage mesoporous biochar material |
| CN115041015A (en) * | 2022-06-22 | 2022-09-13 | 广东工业大学 | Method for removing VOCs (volatile organic compounds) by using water vapor activated persulfate semidry method and application thereof |
Citations (1)
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| CN105776177A (en) * | 2016-03-11 | 2016-07-20 | 北京化工大学 | Laminar boron-doped ordered mesoporous carbon and preparation method thereof |
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- 2017-07-11 CN CN201710559414.1A patent/CN107175093A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105776177A (en) * | 2016-03-11 | 2016-07-20 | 北京化工大学 | Laminar boron-doped ordered mesoporous carbon and preparation method thereof |
Non-Patent Citations (2)
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| XIAOCHEN ZHAO, ET AL.: "Decorated resol derived mesoporous carbon: highly ordered microstructure, rich boron incorporation, and excellent electrochemical capacitance", 《RSC ADVANCES》 * |
| XIAOGUANG DUAN, ET AL.: "Effects of nitrogen-, boron-, and phosphorus-doping or codoping on metal-free graphene catalysis", 《CATALYSIS TODAY》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110302769A (en) * | 2018-03-20 | 2019-10-08 | 中国科学院大连化学物理研究所 | A kind of catalyst carrier, loaded catalyst and its preparation method and application |
| CN110652978A (en) * | 2019-08-27 | 2020-01-07 | 浙江理工大学 | Preparation method and application of nonmetal modified carbon fiber |
| CN112441659A (en) * | 2019-08-30 | 2021-03-05 | 湖南大学 | Method for degrading and treating organic pollutants by activating persulfate through multi-stage mesoporous biochar material |
| CN111111637A (en) * | 2019-12-31 | 2020-05-08 | 太原理工大学 | Boron-doped non-metallic catalyst and preparation method and application thereof |
| CN111450865A (en) * | 2020-04-28 | 2020-07-28 | 中山大学 | Preparation method and application of catalyst for oxidative degradation of bisphenol A by sulfate radical |
| CN111450865B (en) * | 2020-04-28 | 2021-06-11 | 中山大学 | Preparation method and application of catalyst for oxidative degradation of bisphenol A by sulfate radical |
| CN115041015A (en) * | 2022-06-22 | 2022-09-13 | 广东工业大学 | Method for removing VOCs (volatile organic compounds) by using water vapor activated persulfate semidry method and application thereof |
| CN115041015B (en) * | 2022-06-22 | 2023-09-22 | 广东工业大学 | Method for removing VOCs (volatile organic compounds) by using water vapor activated persulfate semi-dry method and application thereof |
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