CN105540819B - A kind of method of support modification preparation ozone catalyst processing organic wastewater with difficult degradation thereby - Google Patents
A kind of method of support modification preparation ozone catalyst processing organic wastewater with difficult degradation thereby Download PDFInfo
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- CN105540819B CN105540819B CN201610066943.3A CN201610066943A CN105540819B CN 105540819 B CN105540819 B CN 105540819B CN 201610066943 A CN201610066943 A CN 201610066943A CN 105540819 B CN105540819 B CN 105540819B
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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
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
-
- 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
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
-
- 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
-
- 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
Abstract
A kind of method of support modification preparation ozone catalyst processing organic wastewater with difficult degradation thereby, belongs to the method for processing organic wastewater with difficult degradation thereby.Method: (1) activation processing of carrier: the active carbon bought is cleaned with deionized water, later with boiling water boiling about 2 hours, then is washed till neutrality, dry；(2) carrier the modification of carrier: is subjected to supersonic modifying；(3) loaded catalyst the preparation of catalyst: is prepared using the method that dipping-precipitated phase combines；Modified active carbon is immersed in manganese nitrate solution, and sodium hydroxide solution is added dropwise in dipping in shaking table, and oscillation filtering precipitating, dry in shaking table, is put into drier after cooling；(4) joint ozone oxidation removes organic wastewater with difficult degradation thereby: the phenolic waste water of 100mg/l being carried out catalytic ozonation, selects optimal catalyst modification mode in conjunction with the removal ability of phenol.Advantage: change absorbent charcoal carrier surface characteristic and pore structure using ultrasound, the load capacity of fortifying catalytic agent handles hardly degraded organic substance significant effect.
Description
Technical field
The present invention relates to a kind of method for handling organic wastewater with difficult degradation thereby, especially a kind of support modification prepares ozone catalytic
The method of agent processing organic wastewater with difficult degradation thereby.
Background technique
Organic wastewater with difficult degradation thereby refers to, and speed is very slow when being decomposed by the microorganisms, and decomposing halfway organic matter (also includes certain
The metabolite of a little organic matters), have the characteristics that toxicity is big, complex in composition, chemical oxygen consumption (COC) is high, biodegradability is poor, is current
The hot spot and difficult point of water prevention and cure of pollution research.In recent years, using advanced oxidation processes handle such waste water research it is more, because of its energy
The extremely strong hydroxyl radical free radical of oxidability is generated, can effectively decompose toxic, bio-refractory organic pollutants, or even thoroughly
Mineralising has the advantages that oxidisability is strong, operating condition is easily controllable.Wherein, ozone oxidation effectively destroys unsaturated knot because having
Structure, it is without secondary pollution the features such as, by the favor of numerous researchers, and heterogeneous catalysis ozonation technique, be catalyzed oxygen improving
The outstanding advantages of change efficiency, reduce catalyst loss, improve catalyst service life etc., become ozonation technology
The new hot spot of research.
In the selection of heterogeneous ozone catalytic agent carrier, active carbon especially more flourishing with relative low price, hole
It is in the majority.For the load capacity of fortifying catalytic agent, there is researcher to inquire into and start with from the surface characteristic for changing active carbon, to activity
Charcoal carries out the modes such as sour modification, alkali modification, oxidation modification, improves catalytic ozonation organic wastewater with difficult degradation thereby to a certain extent
Performance.However, the active carbon as porous material, compared to the active sites that surface can be used for adsorbing simultaneously supported catalyst
Point, specific surface area and active site that huge internal void has will be cannot be neglected, and the contents of the section at present
Research is related to less.
Summary of the invention
The invention aims to provide a kind of catalytic ozonation organic wastewater with difficult degradation thereby processing capacity of capable of significantly improving
The method that support modification prepares ozone catalyst processing organic wastewater with difficult degradation thereby.
The object of the present invention is achieved like this: the method for the processing organic wastewater with difficult degradation thereby: changing activity using ultrasound
Carbon surface characteristic and pore structure, enhancement activated carbon surface-active site and internal void are adsorbed and are loaded to metallic catalyst
Ability, reinforcement, catalysis and ozonization hardly degraded organic substance, the specific steps are as follows:
(1) activation processing of carrier: the active carbon bought is cleaned with deionized water, later with boiling water boiling about 2 hours, then
It is washed till neutrality, 105 DEG C of dryings；
(2) modification of carrier: carrying out supersonic modifying for carrier, select the ultrasonic power of supersonic modifying for 75~150w, surpasses
Acoustic frequency is 50~55Hz, and ultrasonic time is 30~90min, and the surface characteristic and pore structure to active carbon are modified；
(3) loaded catalyst the preparation of catalyst: is prepared using the method that dipping-precipitated phase combines；Modified 5g
Active carbon is immersed in manganese nitrate (AR) solution of 100ml 5%, is impregnated in 150~180r/min shaking table at least for 24 hours, Zhi Houhuan
Slow sodium hydroxide (AR) solution that 1~3mol/l of 45ml is added dropwise, and 1~2h is vibrated in shaking table, filtering precipitates later, and
105~120 DEG C of dry 12h in baking oven, the sample after drying dry 3h in 500~700 DEG C of Muffle furnaces, are put into drying after cooling
It is spare in device；
(4) joint ozone oxidation removes target organic wastewater: the phenolic waste water of 100mg/l is carried out catalytic ozonation, knot
The removal ability for closing phenol, selects the catalyst effect through the modified preparation of ultrasound 60min or so under the conditions of 150W, 53Hz most
It is excellent；The solution PH of the catalytic ozonation is 9~11, and ozone dosage is 3~7mg/l.
The selected carrier of the step (1) is rodlike active carbon.
The step (2) determines ultrasound to the optimal conditions of support modification: ultrasound 60min under the conditions of 150W, 53Hz.
Step (3) load solution used is manganese nitrate solution.
The phenolic waste water concentration that the step (4) is chosen is 100mg/l, and solution PH is 10, and ozone dosage is 6.12mg/
l。
Beneficial effect, due to using above-mentioned support modification scheme, the rodlike active carbon cost of investment of selection is low and is not easy
It is lost, active carbon strengthens the adsorption effect of catalyst after modification, catalytic effect and other method of modifying
Compared to significantly improving.The surface of carrier and pore characteristic are modified by ultrasound, improve the absorption of catalyst and born
Loading capability, using high vacuum mode image acquisition+energy spectrum analysis surface analysis mode (EDS) analysis shows: the load of non-supersonic modifying
Manganese element is 2.40%, and the content of modified manganese element is 3.95%, and the content of sonicated rear impurity element has
A degree of reduction；There is the effect of catalytic ozonation phenol after support modification is obviously improved: 150W, 53KHz, 60min's is super
Under the conditions of sound, the removal rate of 33min phenol improves 34.11% up to 85.78%, than not modified, than alkali modification, Nitric Acid Modified and
Hydrochloric Acid Modification is respectively increased 11.73%, 14.22% and 22.75%.The present invention not only changing based on activated carbon surface characteristic
Become, be more conceived to the change of active carbon internal pore structure, plays active carbon huge internal void and metallic catalyst is adsorbed
And load capacity, under optimal conditions, the degradation property significant effect of rear target organic wastewater is combined with ozone oxidation.
Advantage: cost is relatively low for the method to organic wastewater with difficult degradation thereby, changes it using more universal active carbon and ultrasound
Surface characteristic and pore structure, modified active carbon strengthen the absorption of catalyst and load effect, catalytic ozonation
Hardly degraded organic substance effect is significantly increased compared with unmodified and other method of modifying.
Detailed description of the invention:
Fig. 1 a is the scanning electron microscope (SEM) photograph of the invention without supersonic modifying Supported Manganese.
Fig. 1 b is the scanning electron microscope (SEM) photograph of supersonic modifying back loading manganese of the invention.
Fig. 2 a is the EDS energy spectrum diagram after not sonicated activated carbon supported manganese.
Fig. 2 b is the manganese element mapping after not sonicated activated carbon supported manganese.
Fig. 2 c is the EDS energy spectrum diagram after supersonic modifying after activated carbon supported manganese.
Fig. 2 d is the manganese element mapping after supersonic modifying after activated carbon supported manganese.
Fig. 3 is the catalytic ozonation effect picture of different carriers modification mode of the invention.
Fig. 4 is the catalytic ozonation effect picture of different ultrasonic power modified support of the invention.
Fig. 5 is the catalytic ozonation effect picture of different ultrasonic time modified supports of the invention.
Fig. 6 a is the scanning electron microscope (SEM) photograph of the invention without supersonic modifying active carbon.
Fig. 6 b is the scanning electron microscope (SEM) photograph of active carbon after supersonic modifying of the invention.
Specific embodiment
The method of the processing organic wastewater with difficult degradation thereby: utilizing ultrasonic directed change activated carbon surface characteristic and pore structure,
To metallic catalyst absorption and load capacity, reinforcement, catalysis and ozonization is difficult for enhancement activated carbon surface-active site and internal void
Degradation of organic substances, the specific steps are as follows:
(1) activation processing of carrier: the active carbon bought is cleaned with deionized water, later with boiling water boiling about 2 hours, then
It is washed till neutrality, 105 DEG C of dryings；
(2) modification of carrier: carrying out supersonic modifying for carrier, select the ultrasonic power of supersonic modifying for 70~150w, surpasses
Acoustic frequency is 50~55Hz, and ultrasonic time is 30~90min, and the surface characteristic and pore structure to active carbon are modified；
(3) loaded catalyst the preparation of catalyst: is prepared using the method that dipping-precipitated phase combines；Modified 5g
Active carbon is immersed in manganese nitrate (AR) solution of 100ml 5%, is impregnated in 150~180r/min shaking table at least for 24 hours, Zhi Houhuan
Slow sodium hydroxide (AR) solution that 1~3mol/l of 45ml is added dropwise, and 1~2h is vibrated in shaking table, filtering precipitates later, and
105~120 DEG C of dry 12h in baking oven, the sample after drying are dried 3~4h in 500~700 DEG C of Muffle furnaces, are put into after cooling
It is spare in drier；
(4) joint ozone oxidation removes target organic wastewater: the phenolic waste water of 100mg/l is carried out catalytic ozonation, knot
The removal ability for closing phenol selects optimal improved catalysts；The solution PH of the catalytic ozonation is 9~11, and ozone is thrown
Dosage is 3~7mg/l.
The selected carrier of the step (1) is rodlike active carbon.
The step (2) determines ultrasound to the optimal conditions of support modification: ultrasound 60min under the conditions of 150W, 53Hz, and benefit
Hold pore diameter characteristics with the surface characteristic, specific surface area and hole that scanning electron microscope and surface analyzer characterization prepare rear catalyst.
Step (3) load solution used is manganese nitrate solution.
The phenolic waste water concentration that the step (4) is chosen is 100mg/l, and solution PH is 10, and ozone dosage is 6.12mg/
l。
For that can further appreciate that the contents of the present invention, feature and effect, specific experimental program is hereby enumerated, and cooperate chart
The present invention will be described in detail.
Embodiment 1: a kind of method that support modification prepares heterogeneous ozone catalyst intensive treatment organic wastewater with difficult degradation thereby,
The modification of activation processing, carrier including carrier, the preparation of catalyst, joint ozone oxidation remove target waste water step, including
Following specific steps:
(1) activation processing of carrier: the active carbon bought is cleaned with deionized water, later with boiling water boiling about 2 hours, then
It is washed till neutrality, 105 DEG C of dryings.
(2) modification of carrier: supersonic modifying: select the ultrasonic power of supersonic modifying for 75w, 112.5w, 150w, supersonic frequency
Rate is 53Hz, and then selects the ultrasonic time of supersonic modifying for 30min, 40min, 50min, 60min, 75min, 90min；150w
Under ultrasound condition, the surface characteristic and pore structure to active carbon are modified, table 1.
1 supersonic modifying of table
Compare simultaneously with other surfaces modification mode: 1. acid is modified: dilute salt that configuration 100ml mass fraction is 2%
Acid weighs 10g active carbon and impregnates wherein, is put into baking oven and is dried for standby after dipping 5h at 45 DEG C；2. alkali modification: configuration 100ml
The sodium hydroxide that mass fraction is 2% weighs 10g active carbon and impregnates wherein, 5h is impregnated at 45 DEG C, is dried for standby in baking oven；③
Oxidation modification: active carbon being placed in the nitric acid solution that 100ml mass fraction is 5%, and 2h is impregnated at 60 DEG C and is modified, later
It is cleaned with pure water, is dried at 105 DEG C.
(3) manganese type carbon base catalyst the preparation of catalyst: is prepared using the method that dipping-precipitated phase combines；It will be modified
5g active carbon be immersed in the manganese nitrate solution of 100ml 5%, impregnated in 180r/min shaking table for 24 hours, hydroxide be added dropwise later
Sodium solution stirs 1h, filtering precipitating, and dries 12h in an oven, and the sample after drying is dry in 500~700 DEG C of Muffle furnaces
3h is put into spare in drier after cooling；
(4) combine ozone oxidation target organic wastewater: taking 100mg/l phenolic waste water 1L, adjusting PH is 10, ozone dosage
For 6.12mg/l, 2g catalyst is added in waste water and carries out, is tested, 0min, 5min, 10min, 15min, 20min,
It is sampled respectively in sample tap when 25min, 30min, phenol concentration is measured using visible spectrophotometer, calculates the removal of phenol
Rate.
As seen from Table 1, specific surface area and hole are melted aperture and are changed before and after support modification, are ultrasonically treated 30min
When middle, BET specific surface area, hole are melted aperture and are declined slightly, and the ash content and impurity of part are also remained in pretreated active carbon,
The tiny group and impurity that carrier surface has further been stripped by being ultrasonically treated, make more to clean in its surface and hole, make
Micropore gradually displays, and aperture is reduced；When ultrasonic 60min, specific surface area increases, and aperture is melted in hole to be had with regard to 30min ratio
Increase, with the proper extension of time, cavitation becomes strong, and percussion makes partial pore be broken into mesoporous, wherein mesoporous
Conveying effect is played, adsorption rate is dominate, mesoporous increases the suction-operated for enhancing active carbon, more preferable convenient for active component
Dispersion and deposition；But when arriving 90min, specific surface area and hole are melted aperture and are declined, this is because intense impact action breaks down
Hole wall, causes amount of activated charcoal mechanism to collapse, partial hole ruptures.Therefore, when comprehensively considering in this research using ultrasound
Between 60min be optimum carrier modified condition.
In Fig. 3, Fig. 4 and Fig. 5, the ability of catalytic ozonation target waste water is it is found that carry out ultrasound to absorbent charcoal carrier in figure
Modified, the removal of ultrasonic power and target waste water is proportional within the scope of the 75w-150w that this experiment is investigated, in ultrasonic function
Under the conditions of rate is 150w, supersonic frequency is 53Hz, change carrier ultrasonic time, the results showed that prepare through 60min supersonic modifying
Catalyst is best to the degradation property of target organic.
Fig. 6 a and Fig. 6 b are of the invention without supersonic modifying and by the scanning electron microscope (SEM) photograph of supersonic modifying active carbon, can be with
Find out that the active carbon pore size distribution without supersonic modifying is less, and stacks serious, the modified active carbon surface handled through ultrasonic 60min
It more cleans, there is certain stereovision, hole is opposite to increase, mostly through-hole, to illustrate that ultrasound has reached cleaning surface and pore-creating
Purpose.
Embodiment 2: in the method and step:
(2) modification of carrier: carrying out supersonic modifying for carrier, and selecting the ultrasonic power of supersonic modifying is 75, supersonic frequency
For 53Hz, ultrasonic time 90min；
(3) loaded catalyst the preparation of catalyst: is prepared using the method that dipping-precipitated phase combines；Modified 5g
Active carbon is immersed in manganese nitrate (AR) solution of 100ml 5%, is impregnated in 150~180r/min shaking table at least for 24 hours, Zhi Houhuan
Slow sodium hydroxide (AR) solution that 1~3mol/l of 45ml is added dropwise, and 1~2h is vibrated in shaking table, filtering precipitates later, and
105 DEG C of dry 12h in baking oven, the sample after drying are dried 4h in 500 DEG C of Muffle furnaces, are put into after cooling spare in drier；
(4) joint ozone oxidation removes target organic wastewater: the phenolic waste water of 100mg/l is carried out catalytic ozonation, knot
The removal ability for closing phenol selects optimal improved catalysts；The solution PH of the catalytic ozonation is 9, ozone dosage
For 7mg/l.
It is other same with embodiment 1.
Embodiment 3: in the method and step:
(2) modification of carrier: carrier is subjected to supersonic modifying, selects the ultrasonic power of supersonic modifying for 150w, supersonic frequency
Rate is 53Hz, ultrasonic time 30min；
(3) loaded catalyst the preparation of catalyst: is prepared using the method that dipping-precipitated phase combines；Modified 5g
Active carbon is immersed in manganese nitrate (AR) solution of 100ml 5%, is impregnated in 150~180r/min shaking table at least for 24 hours, Zhi Houhuan
Slow sodium hydroxide (AR) solution that 1~3mol/l of 45ml is added dropwise, and 1~2h is vibrated in shaking table, filtering precipitates later, and
120 DEG C of dry 12h in baking oven, the sample after drying are dried 3h in 700 DEG C of Muffle furnaces, are put into after cooling spare in drier；
(4) joint ozone oxidation removes target organic wastewater: the phenolic waste water of 100mg/l is carried out catalytic ozonation, knot
The removal ability for closing phenol selects optimal improved catalysts；The solution PH of the catalytic ozonation is 11, and ozone adds
Amount is 3mg/l.
Other are same with embodiment 1.
Claims (3)
1. a kind of method of support modification preparation ozone catalyst processing organic wastewater with difficult degradation thereby, it is characterized in that: the processing difficulty drops
The method for solving organic wastewater: change activated carbon surface characteristic and pore structure, enhancement activated carbon surface-active site using ultrasound
With internal void to metallic catalyst absorption and load capacity, reinforcement, catalysis and ozonization hardly degraded organic substance, specific steps are such as
Under:
(1) activation processing of carrier: the active carbon bought is cleaned with deionized water, is used boiling water boiling 2 hours later, then be washed till
Property, 105 DEG C of dryings；
(2) modification of carrier: carrier is subjected to supersonic modifying, selects the ultrasonic power of supersonic modifying for 75 ~ 150w, supersonic frequency
For 50 ~ 55Hz, ultrasonic time is 30 ~ 90min, and the surface characteristic and pore structure to active carbon are modified；
(3) loaded catalyst the preparation of catalyst: is prepared using the method that dipping-precipitated phase combines；Modified 5g activity
Charcoal is immersed in the manganese nitrate AR solution of 100ml 5%, is impregnated in 150 ~ 180r/min shaking table at least for 24 hours, is slowly added dropwise later
The sodium hydroxide AR solution of 1 ~ 3mol/l of 45ml, and 1 ~ 2h is vibrated in shaking table, filtering precipitating later, and in an oven 105 ~
1200C dries 12h, and the dry 3 ~ 4h in 500 ~ 700 DEG C of Muffle furnaces of the sample after drying is put into spare in drier after cooling；
(4) joint ozone oxidation removes target organic wastewater: the phenolic waste water of 100mg/l being carried out catalytic ozonation, in conjunction with benzene
The removal ability of phenol selects optimal improved catalysts；The pH value of solution of the catalytic ozonation is 9 ~ 11, ozone dosage
For 3 ~ 7mg/l.
2. a kind of method of support modification preparation ozone catalyst processing organic wastewater with difficult degradation thereby according to claim 1,
It is characterized in that: the selected carrier of the step (1) is rodlike active carbon.
3. a kind of method of support modification preparation ozone catalyst processing organic wastewater with difficult degradation thereby according to claim 1,
It is characterized in that: the step (2) is to determine that ultrasound carries out table to the optimal conditions of support modification, and to the catalyst after preparation
Sign.
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| CN102049253A (en) * | 2009-10-28 | 2011-05-11 | 中国石油化工集团公司 | Preparation method of special catalyst for waste water treatment by ozone oxidation |
| CN102091619A (en) * | 2010-11-23 | 2011-06-15 | 广东工业大学 | Preparation method for ozone catalytic oxidation catalyst and device using catalyst |
| CN102600850A (en) * | 2012-01-13 | 2012-07-25 | 昆明理工大学 | Method for preparing catalyst capable of being subjected to carbon oxysulfide removal and carbon disulfide removal simultaneously |
| CN102600861A (en) * | 2012-03-26 | 2012-07-25 | 中国科学院生态环境研究中心 | Manganese-based composite oxide catalyst for catalytically decomposing ozone, and preparation method of manganese-based composite oxide catalyst |
| CN103739043A (en) * | 2013-09-06 | 2014-04-23 | 广西大学 | Particle electrode for photocatalytic three-dimensional electrode/electro-Fenton system and preparation method thereof |
| CN103586026A (en) * | 2013-11-26 | 2014-02-19 | 北京碧水源科技股份有限公司 | Carbon supported catalyst for ozone oxidation, and preparation method and use thereof |
| CN104261504A (en) * | 2014-09-16 | 2015-01-07 | 同济大学 | Method for removing sulfamethoxazole in water body by using modified bamboo charcoal |
| CN105080565A (en) * | 2015-06-03 | 2015-11-25 | 博天环境集团股份有限公司 | Method for preparing supported ozone oxidation catalyst |
| CN105001155A (en) * | 2015-09-04 | 2015-10-28 | 南通职业大学 | Oxosynthesis method of methylpyridine-1-oxide |
| CN105233855A (en) * | 2015-11-16 | 2016-01-13 | 建德市环保科技创新创业中心有限公司 | Zeolite loading catalyst, preparation method thereof and application thereof to organic wastewater treatment |
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