CN106378127A - A NaClO oxidation catalyst used for deep treatment of industrial waste water, a preparing method thereof and applications of the catalyst - Google Patents
A NaClO oxidation catalyst used for deep treatment of industrial waste water, a preparing method thereof and applications of the catalyst Download PDFInfo
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- CN106378127A CN106378127A CN201610695691.0A CN201610695691A CN106378127A CN 106378127 A CN106378127 A CN 106378127A CN 201610695691 A CN201610695691 A CN 201610695691A CN 106378127 A CN106378127 A CN 106378127A
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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
- 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
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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
- 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
- B01J23/20—Vanadium, niobium or tantalum
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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
-
- 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
- C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
Abstract
The invention relates to a NaClO oxidation catalyst used for deep treatment of industrial waste water, a preparing method thereof and applications of the catalyst. The catalyst comprises a carrier and an active component, wherein the carrier is at least one of at least one of Al2O3, MgO and diatomite, the active component is at least one of oxides of Mn, Ti, V and Ta and is loaded in a manner of nanorods or/and nanoparticles onto the carrier, and the mass of the active component is 5-50% of the total mass of the catalyst. The catalyst is used together with NaClO, has excellent degradation capabilities for a plurality of pollutants such as pollutants represented by COD and ammonia nitrogen, and has excellent decoloration effects.
Description
Technical field
The present invention relates to a kind of catalyst and preparation method thereof, concretely relate to a kind of sewage disposal NaClO oxygen
Change catalyst and preparation method thereof.
Background technology
For the increasingly serious problem of water pollution, the requirement to industrial wastewater discharge for the China is more and more strict, current emphasis
The industrial wastewater discharge standard in the area such as basin such as Yangtze River Delta improves to one-level A standard from one-level B before 1 day January in 2015,
As COD (COD) discharge standard brings up to below 50mg/L from below 60mg/L, Aniline categories in dyeing waste water
Discharge standard must not bring up to from 1mg/L and detect (＜ 0.03mg/L).Thus each commercial production enterprise and whole sewage disposal
Industry all suffers from a difficult problem for urgent technological innovation and industrial upgrading.
However, requiring with respect to increasingly stricter sewage discharge, the advanced treatment of wastewater technology of current high efficiency, low cost
But it is short of very much, do not have big breakthrough always.High-level oxidation technology is the most effectual way realizing advanced treatment of wastewater, such as
Fenton, ozone, photocatalysis etc..But these traditional advanced oxidization methods have many shortcomings in actual applications.
Fenton and photocatalytic oxidation are the oxidation technologies based on hydroxyl radical free radical (OH), and its essence is that OH passes through
The approach such as electron transfer, electrophilic addition, dehydrogenation reaction make the various pollutant mineralisings in water, make harmful substance be degraded to CO2、H2O
With other inorganic substances, or the intermediate product being translated into low toxicity easily biological-degradable.Wherein photocatalytic oxidation passes through to excite
TiO2To produce OH, the method subject matter is that transmission journey in water for the light is shorter and TiO2Need ultraviolet excitation, above-mentioned
Reason leads to reactor to need particular design, equipment and operating cost all higher, thus the method is also difficult at trade effluent
Practical application is obtained in science and engineering journey；Fenton oxidation method typically just can be carried out in acid condition, substantial amounts of due to needing to add
Fe2+And H2O2Medicament, can produce a large amount of mud, increased the difficulty of after-treatment.In addition, the above-mentioned oxygen based on hydroxyl radical free radical
The disadvantage changing processing method is when there is inorganic ionss (PO in water4 3-、Cl-、HCO3 -、CO3 2-) when, inorganic ionss will
Produce competitive reaction with OH and total chemical oxygen consumption (COC) (COD) clearance is reduced.
Other advanced oxidization methods are also difficult to because of the problem being individually present extensively apply, such as catalytic wet air oxidation due to
Using high pressure, high temperature harsh conditions and noble metal catalyst, therefore relatively costly；It is oxidation that Ozonation mainly utilizes ozone
Agent, but ozone utilization rate is low and selectivity is poor, and equipment cost and operating cost are all very high；Electrochemical process efficiency is low, high energy consumption,
Economically unreasonable；Based on potentiometric titrations (SO4 -) the place to hardly degraded organic substance for the persulfate high-level oxidation technology
Reason is not thorough, and the reaction required time is longer；Potassium ferrate oxidizing process reagent cost is too high, and has mud generation simultaneously.
NaClO is the by-product of chlorine industry, has the characteristics that with low cost.It has in acidity and weakly alkaline solution
Compared with strong oxidizing property, and have the advantages that cheap, sterilizing ability is strong, be easy to produce and become a kind of conventional wastewater treatment
Agent.But sodium hypochlorite is limited to the Oxidation of persistent organic pollutants, its treatment effect generally not as good as ozone oxidation,
The methods such as Fenton.
For lifting the oxidability to Recalcitrant chemicals in water for the NaClO, researchers find using having variable valency
Transition metal oxide is catalyst, can be catalyzed NaClO generation and have higher active elemental oxygen, thus realize difficult degradation having
The depth degradation of organic pollutants.But, with Co, Ni as main component, price is very high for the associated catalysts of domestic and international report at present
Expensive.On the other hand, for avoiding the molten damage of active component, the work pH of this kind of catalyst is higher, usually 9-14, and this may lead
Cause Ca in water2+It is deposited and is attached to catalyst surface Deng with insoluble matter form, thus reduce its catalytic efficiency shortening urging
Agent service life.
Content of the invention
For a difficult problem for hardly degraded organic substance process up to standard in above-mentioned trade effluent, it is an object of the invention to provide a kind of
NaClO oxidation catalyst with low cost and preparation method thereof, to reach efficient, inexpensive degraded COD, realizes one-level A up to standard
The purpose of discharge.
On the one hand, the invention provides a kind of NaClO oxidation catalyst, described NaClO oxidation catalyst includes Al2O3、
At least one in MgO, kieselguhr be carrier, and in the form of nanometer rods or/and nanoparticle uniform load in described load
At least one in the oxide of Mn, Ti, V, Ta of body is active component, and it is total that described active component accounts for NaClO oxidation catalyst
The percentage ratio of quality is 5～50%.
It is preferred that a diameter of 10～100nm of described nanoparticle, or/and the length of described nanometer rods be 80～
150nm, draw ratio are 3～10.
On the other hand, present invention also offers a kind of preparation method of NaClO oxidation catalyst, including：
By carrier impregnation in the precursor solution of described active component, obtain catalyst precursor after drying；
Gained catalyst precursor is placed under air in Muffle furnace in 300～550 DEG C of roastings, obtains described NaClO oxidation and urge
Agent.
It is preferred that the precursor solution of described active component is Mn (NO3)2Solution, tetrabutyl titanate solution, ammonium vanadate are molten
At least one in liquid, ethanol tantalum solution.
Also, it is preferred that in the precursor solution of described active component metal ion total concentration be 1～8mol/L.
It is preferred that described dipping is to impregnate 6～24 hours at 5～50 DEG C.
It is preferred that described drying is to be dried 2～24 hours at 50～140 DEG C.
It is preferred that described being roasted to sinters 2～8 hours at 300～550 DEG C.
Another further aspect, the invention provides a kind of NaClO oxidation catalyst answering in NaClO advanced treatment of industrial wastewater
With.
The present invention mainly has the advantages that：
The catalyst of present invention preparation does not contain rare precious metal, thus cost is relatively low；
Method for preparing catalyst process is simple according to the present invention, without expensive device it is easy to large-scale production；
Catalyst activity is very high, and catalytic oxidation speed quickly, is typically reacted complete in 5-15min, dirt is no longer detected
Dye thing concentration change；
The NaClO oxidation catalyst of present invention preparation is used in conjunction with NaClO, and multiple pollutant such as COD, ammonia nitrogen etc. are respectively provided with
Excellent degradation capability, also has excellent decolorizing effect simultaneously.
The NaClO oxidation catalyst of the present invention can be obviously improved NaClO to the disposal ability of persistent organic pollutants and
Oxidation reaction speed, performance projects and wide accommodation, thus can be applicable to least significant end advanced treatment process, is widely used in stone
One-level A of the industry wastewater treatments such as oiling work, Coal Chemical Industry, oilfield exploitation, food, timber processing proposes mark transformation.
Brief description
Fig. 1 is the SEM photograph of the alumina load manganese oxide catalyst of embodiment 1 preparation；
Fig. 2 is the decolorizing effect figure to redwood processing waste water for the tripolite loading manganese oxide catalyst of embodiment 3 preparation.
Fig. 3 is the SEM photograph of the alumina load tantalum oxide catalyst of embodiment 5 preparation.
Specific embodiment
Further illustrate the present invention below by way of following embodiments it should be appreciated that following embodiment is merely to illustrate this
Invention, and the unrestricted present invention.
The present invention is directed to the difficult problem that persistent organic pollutants biodegradability is poor, processing cost is high, is prepared for one kind and is based on
The new catalytic material of reactive metal oxides, can efficient organic pollution in advanced treatment of industrial wastewater.Catalyst carrier
For Al2O3, MgO, the porous mass such as kieselguhr, active component be one of oxide of transition metal such as Mn, Ti, V, Ta or
Several, and in the form of nanometer rods or/and nanoparticle uniform load on described carrier.Catalyst is according to active component and preparation
Method difference can be nanometer rods or/and nanoparticle form.Wherein, the length of described nanometer rods is about 80-150nm, draw ratio
For 3～10.The diameter of described nanoparticle is about 10～100nm.
The preparation method of the NaClO oxidation catalyst that the explanation present invention in following exemplary ground provides.
By carrier impregnation (for example, impregnating 6～24 hours at 5～50 DEG C) in the precursor solution of described active component
In, obtain catalyst precursor after drying (for example, being dried 2～24 hours at 50～140 DEG C).Wherein said active component
Precursor solution can be Mn (NO3)2In the solution such as solution, tetrabutyl titanate solution, Ammonium Vanadate Solution, ethanol tantalum solution extremely
Few one kind.Such as Mn (NO3)2Solution is aqueous solution, the ethanol solution of tetrabutyl titanate, the ethanol solution of ammonium vanadate, ethanol tantalum
Ethanol solution etc..Additionally, the total concentration of metal ion need to reach 1～8mol/L in the precursor solution of described active component.
Catalyst precursor is placed under air in Muffle furnace in 300～550 DEG C of roastings, naturally cools to room temperature, obtain final product
To advanced treatment of industrial waste water NaClO oxidation catalyst.Wherein, described roasting can be little in 300～550 DEG C of sintering 2～8
When.
The catalyst of present invention preparation does not use rare precious metal, thus cost is relatively low, and it is high, steady to have normal-temperature reaction activity
The advantages of qualitative height, long service life.The present invention preparation NaClO oxidation catalyst except oxidation reaction speed can be improved,
NaClO oxidability can also be improved, some pollutant that individually cannot be aoxidized with NaClO, urged using NaClO+NaClO oxidation
Agent then can aoxidize.Such as, the pollutant such as COD, ammonia nitrogen are respectively provided with excellent treatment effect, and there is excellent decolouring effect
Really.
Present invention also offers a kind of application in NaClO advanced treatment of industrial wastewater for NaClO oxidation catalyst.
NaClO oxidation catalyst prepared by the present invention is combined with NaClO common degraded industrial wastewater.Wherein NaClO
The addition of oxidation catalyst is 0.01-10g/L waste water, and the addition of corresponding NaClO can be 0.01-50g/L waste water,
And adjusted its pH value to 9-11 using dilute sulfuric acid, now catalysis activity height and effect stability.Catalysis using present invention preparation
Agent, only needs hypochlorite oxidation to process 5-15min, you can to realize electroplating sewerage, coal chemical industry sewage, food processing sewage, timber
The COD one-level A qualified discharge of the polytype waste water such as processing sewage.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this
Some nonessential improvement that bright the above is made and adjustment belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only one of OK range example, and that is, those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
By 100g alumina support mass concentration be 50% six water manganese nitrate solutions in impregnate 12h, drip only after naturally dries；
Then it is dried 15 hours at 120 DEG C, be placed in roasting 3 hours at 450 DEG C in Muffle furnace, finally give being loaded with of this test
The catalyst of manganese oxide, burning till manganese oxide percentage composition in rear sample is 50%.Fig. 1 is the SEM photograph of the catalyst of preparation, can
See, MnO2Present bar-shaped, length is about 100nm, draw ratio is between 5-10, and is equably supported on the alumina support of porous
On.
The manganese oxide catalyst of above-mentioned for 6g alumina load is added 100mL to first pass through the plating of two-stage Fenton process in advance
In waste water, add the NaClO aqueous solution that 0.6mL mass concentration is 10%, plus several dilute H2SO4PH value is adjusted to 8.0, shaking table
Upper 100rpm reacts 1h.Before catalytic treatment, electroplating wastewater COD is 85mg/L, waste water COD after above-mentioned NaClO catalytic oxidation treatment
For 28mg/L.Using same reaction conditions, it is added without catalyst, and process waste water only with NaClO solution, in processed waste water
COD concentration is 67mg/L, continues to extend the response time to 2h, COD is held essentially constant it is impossible to reach one-level A emission request
(COD ＜ 50mg/L).Above-mentioned the results show, the catalyst of present invention preparation can significantly increase sodium hypochlorite in waste water
The oxidation effectiveness of persistent organic pollutants, realizes electroplating wastewater COD one-level A qualified discharge.
Embodiment 2
By 100g diatomite support mass concentration be 50% six water manganese nitrate aqueous solutions in impregnate 12h, drip only after naturally dries in the air
Dry；Then it is dried 15 hours at 120 DEG C, be placed in roasting 6 hours at 400 DEG C in Muffle furnace, finally give the silicon of this test
Diatomaceous earth loads the catalyst of manganese oxide, and burning till manganese oxide percentage composition in rear sample is 30%.MnO2Present bar-shaped, length is about
100nm, draw ratio is between 5-10, and is equably supported on the alumina support of porous.
The manganese oxide catalyst of above-mentioned for 4g tripolite loading is added in 100mL alcohol waste water, adds 0.6mLNaClO molten
Liquid (mass concentration is 10wt%), plus several dilute H2SO4PH value is adjusted to 8.0.After 100rpm reaction 10min on shaking table, ethanol
Waste water COD is down to below 42mg/L by 350mg/L, reaches country-level emission standard A.Contrastingly, do not use catalyst, its
In the case that his reaction condition is identical, after reaction 30min, the COD of alcohol waste water is 150mg/L.Illustrate that catalyst can show
Write the oxidation effectiveness strengthening sodium hypochlorite, realize the advanced treating of organic pollution in alcohol waste water.
Embodiment 3
By 100g diatomite support mass concentration be 50% six water manganese nitrate solutions in impregnate 12h, drip only after naturally dries；
Then in 120 DEG C of dryings 15 hours, it is placed in roasting 6 hours at 400 DEG C in Muffle furnace, finally give the load aerobic of this test
Change the catalyst of manganese, burning till manganese oxide percentage composition in rear sample is 30%.MnO2Present bar-shaped, length is about 100nm, major diameter
Ratio is between 5-10, and is equably supported on the alumina support of porous.
The manganese oxide catalyst of above-mentioned for 4g tripolite loading is added in 100mL redwood processing waste water, adds
0.4mLNaClO solution (mass concentration is 10%), plus several dilute H2SO4PH value is adjusted to 8.0.100rpm reaction on shaking table
After 5min and 10min, separately sampled.After being followed successively by before processing and NaClO catalysis oxidation 5min and 10min in Fig. 2 from left to right
Redwood processing waste water photo.It can be seen that, this catalyst has excellent decolorizing effect to redwood processing waste water.
Embodiment 4
100g Woelm Alumina powder body is added in 200mL butyl titanate (1.5M) and the ethanol solution of ethanol tantalum (0.5M), leaching
Stain is adsorbed 15 hours, naturally dries after drip only；Then it is dried 15 hours at 120 DEG C, be placed in roasting 3 at 450 DEG C in Muffle furnace
Hour, finally give the catalyst of the loading titanium oxide-tantalum oxide of this test.Titanium oxide assumes graininess, a diameter of 10-
30nm.Tantalum oxide presents bar-shaped, and length is about 100nm, and draw ratio is between 5-10, and is equably supported on the aluminium oxide of porous
On carrier.
The titanium oxide of above-mentioned for 6g alumina load-tantalum oxide catalyst is added in 100mL dyeing waste water, adds 0.4mL
Mass concentration is 10% NaClO aqueous solution, plus H2SO4Adjust pH to 9.0,100rpm reaction 20min on shaking table.Before processing is given up
In water, COD content is 120mg/L, and after process, COD is down to 35mg/L, reaches country-level emission standard A.
Embodiment 5
100g alumina support is immersed in the ethanol solution of 1.5M ethanol tantalum, dipping absorption 15 hours, naturally dries in the air after drip only
Dry；Then it is dried 15 hours at 120 DEG C, is placed in roasting 3 hours at 450 DEG C in Muffle furnace, finally give the negative of this test
Carry the catalyst of tantalum oxide, burning till tantalum oxide percentage composition in rear sample is 14.2%.Fig. 3 is that the SEM of the catalyst of preparation shines
Piece is it is seen then that Ta2O5Assume bar-shaped, length 100-150nm, draw ratio is between 3-8, and is equably supported on the aluminium oxide of porous
On carrier.
The tantalum oxide catalyst of above-mentioned for 6g alumina load is added 100mL through the coal liquifaction of coagulation and Fenton process
In waste water, add the NaClO aqueous solution that 0.6mL mass concentration is 10%, plus H2SO4Adjust pH to 8.5, on shaking table, 100rpm is anti-
Answer 15min.In waste water before NaClO catalysis oxidation, COD content is 180mg/L, and after process, COD is down to 32mg/L, reaches country one
Level emission standard A.Contrastingly, this waste water adopts ozone oxidation 15min, and processed waste water COD is 58mg/L.The present invention is described
The catalyst of preparation is better than ozone to the treatment effect of coal liquifaction waste water.
Comparative example 1 only adds NaClO aqueous solution
Reference implementation example 5, in 100mL in the coal liquifaction waste water that coagulation and Fenton are processed, addition 0.6mL mass concentration is
10% NaClO aqueous solution, plus H2SO4Adjust pH to 8.5,100rpm reaction 15min on shaking table.Waste water before NaClO catalysis oxidation
Middle COD content is 180mg/L, and after process, COD is down to 32mg/L.By comparative example 1 compared with Example 5, we understand：With independent
Compared using NaClO processed waste water COD concentration 96mg/L, COD can be down to by being used in conjunction with of catalyst and NaClO
32mg/L.Show that catalyst can be obviously improved the oxidability to pollutant for the NaClO.
Comparative example 2 only adds NaClO oxidation catalyst (the tantalum oxide catalyst of alumina load)
Reference implementation example 5, the tantalum oxide catalyst of above-mentioned for 6g alumina load is added 100mL through coagulation and Fenton process
Coal liquifaction waste water in, plus NaOH adjust pH to 8.5, on shaking table 100rpm reaction 15min.The tantalum oxide catalysis of alumina load
In waste water before agent catalysis oxidation, COD content is 180mg/L, and after process, COD is 160mg/L.By comparative example 2 compared with Example 5
We understand, only add NaClO oxidation catalyst, and the COD concentration after wastewater treatment only reduces 20mg/L, explanation compared with before processing
NaClO catalyst does not have the single ability aoxidizing organic pollution, and COD concentration reduces 20mg/L may be with catalyst
Adsorption is related.
Additionally, in conjunction with the embodiments 5, comparative example 1 and comparative example 2 the data obtained it can be seen that the present invention preparation catalyst
Itself do not have oxidation stain thing ability.But catalyst can be obviously improved the oxidation to persistent organic pollutants for the NaClO
Ability, it is bigger, thus meeting Sewage advanced treatment and one-level A demand up to standard that COD concentration reduces amplitude.
In the present invention, COD is recorded using the DR2800 portable spectrophotometer of HACH company of the U.S..
Claims (9)
1. a kind of NaClO oxidation catalyst is it is characterised in that described NaClO oxidation catalyst includes Al2O3, MgO, in kieselguhr
At least one be carrier, and be carried on Mn, Ti, V, Ta of described carrier in the form of nanometer rods or/and nanoparticle
At least one in oxide be active component, described active component account for NaClO oxidation catalyst gross mass percentage ratio be 5～
50%.
2. NaClO oxidation catalyst according to claim 1 it is characterised in that described nanoparticle a diameter of 10～
100nm, or/and the length of described nanometer rods be 80～150nm, draw ratio be 3～10.
3. a kind of preparation method of NaClO oxidation catalyst as claimed in claim 1 or 2 is it is characterised in that include：
By carrier impregnation in the precursor solution of described active component, obtain catalyst precursor after drying；
Gained catalyst precursor is placed under air in Muffle furnace in 300～550 DEG C of roastings, obtains described NaClO oxidation and urge
Agent.
4. preparation method according to claim 3 is it is characterised in that the precursor solution of described active component is Mn
(NO3)2At least one in solution, tetrabutyl titanate solution, Ammonium Vanadate Solution, ethanol tantalum solution.
5. preparation method according to claim 4 it is characterised in that in the precursor solution of described active component metal from
The total concentration of son is 1～8 mol/L.
6. the preparation method according to any one of claim 3-5 is it is characterised in that described dipping is at 5～50 DEG C
Dipping 6～24 hours.
7. the preparation method according to any one of claim 3-6 is it is characterised in that described drying is at 50～140 DEG C
Lower drying 2～24 hours.
8. the preparation method according to any one of claim 3-7 is it is characterised in that described be roasted at 300～550 DEG C
Sintering 2～8 hours.
9. application in NaClO advanced treatment of industrial wastewater for a kind of NaClO oxidation catalyst as claimed in claim 1 or 2.
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Cited By (1)
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| WO2019200871A1 (en) * | 2018-04-19 | 2019-10-24 | 华南理工大学 | Magnesium-based ferrous sulfide composite nanomaterial, preparation method therefor and use thereof |
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