CN110142043A - The processing method of flyash catalyst, preparation method and organic wastewater - Google Patents
The processing method of flyash catalyst, preparation method and organic wastewater Download PDFInfo
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- CN110142043A CN110142043A CN201910514862.9A CN201910514862A CN110142043A CN 110142043 A CN110142043 A CN 110142043A CN 201910514862 A CN201910514862 A CN 201910514862A CN 110142043 A CN110142043 A CN 110142043A
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/302—Treatment of water, waste water, or sewage by irradiation with microwaves
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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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
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Abstract
The present invention relates to the processing methods of a kind of flyash catalyst, preparation method and organic wastewater.The present invention provides a kind of preparation method of flyash catalyst comprising following steps: will include that flyash is mixed and roasted with the raw material of binder, obtains flyash catalyst.The present invention provides a kind of flyash catalyst, which is prepared by the preparation method.The present invention also provides a kind of processing method of organic wastewater, which includes that microwave catalysis oxidation processing is carried out to organic wastewater, and the catalyst of microwave catalysis oxidation processing is prepared by preparation method of the present invention.Existing active carbon and activated alumina catalyst system are substituted using flyash catalyst of the invention, improve the stability of organic wastewater microwave catalysis system.
Description
Technical field
The present invention relates to catalyst field, in particular to a kind of flyash catalyst, preparation method and organic wastewater
Processing method.
Background technique
Modern chemical industry (such as petrochemical industry, printing and dyeing, pesticide, pharmacy, papermaking, fine chemistry industry, coal oil and coal chemical industry
Industry) a large amount of high concentrations, high toxicity, the organic wastewater containing refractory organic would generally be generated in production process.This
The constituent of a little waste water is complicated, and processing difficulty is big, and if processing will serious ground contamination environment not in time.
Currently, common concentration organic wastewater disposal process mainly has biochemical method, chemical method, physical method, physical chemistry
Method etc..Chemical method mainly has chemical oxidization method, extraction, absorption method, incineration method, catalytic oxidation etc..The big many places of these methods
Complex process is managed, equipment is more, and operation difficulty is big；And since the waste water composition that different process units give off is complicated, cannot concentrate
Processing.Although and bioremediation technique is given birth to compared with mature, equipment is simple, processing capacity is big, operating cost is low for containing hardly possible
Object degradation of organic substances or the waste water for inhibiting biodegradable organic matter, are extremely difficult to good treatment effect.In the 1970s
Start the catalytic wet air oxidation occurred, the high-concentration waste water containing refractory organic can be focused on, but it is needed
It is reacted under high temperature, hyperbaric environment, processing cost is high in practical application, requires the material of reactor high, energy consumption height, largely
On limit its industrial application.
The microwave catalysis oxidation technology that developed recently gets up is a kind of wastewater treatment new method, in normal temperature and pressure or low temperature
It is selectively heated under conditions of low pressure using microwave energy, so that magnetisable material is generated " hot spot ", accelerate the removal of pollutant, it is high in short-term
Effect, it is especially more preferable to the organic pollutant treatment effect of difficult for biological degradation, it has also become to be studied in waste water catalytic oxidation treatment technology
Hot spot, core of the catalyst as catalytic oxidation, even more one of the focus of recent research.Currently, for microwave catalysis
Oxidation catalyst is mostly studied and patent concentrates in active carbon system and activated alumina system, but both are catalyzed
The problems such as system stability is poor, very fast there are catalytic efficiency decline after longtime running or repeatedly reaction, can not be steady in a long-term
Operation, it is difficult to further industrial applications.
Accordingly, it is desirable to provide it is a kind of for handling the catalyst of organic wastewater, it is steady to solve catalyst system in the prior art
Qualitative poor problem.
Summary of the invention
The object of the present invention is to provide the processing method of a kind of flyash catalyst, preparation method and organic wastewater,
To solve the problems, such as that catalyst system stability is poor in the prior art.
To achieve the goals above, according to an aspect of the present invention, the present invention provides a kind of flyash catalyst
Preparation method obtains flyash and urges method includes the following steps: will include that flyash is mixed and roasted with the raw material of binder
Agent.
Further, the weight ratio of flyash and binder is 1~10:1.
Further, the temperature of roasting is 300~900 DEG C, and the time of roasting is 2~24 hours.
Further, before calcination steps, the above method further includes carrying out forming processes to raw material, preferably at the molding
Reason is kneaded and formed；Raw material after molding is dried, the temperature being preferably dried is 80~120 DEG C, at drying
The time of reason is 4~12 hours.
Further, flyash at least contains following component: SiO2、Al2O3、Fe2O3。
Further, binder is that silica solution, Aluminum sol and methylcellulose are any one or more of.
According to another aspect of the present invention, a kind of flyash catalyst is provided, the flyash catalyst is by mentioned earlier
Preparation method of the invention be prepared.
According to another aspect of the present invention, a kind of processing method of organic wastewater is provided, which includes to having
Machine waste water carries out microwave catalysis oxidation processing, the preparation of the invention of the catalyst of microwave catalysis oxidation processing by mentioned earlier
Method is prepared.
Further, the COD value of organic wastewater is 3000~100000.
Further, microwave catalysis oxidation processing includes following process conditions:
Microwave frequency: 400~3000MHz；
Power: 100~5000W；
Reaction temperature: room temperature~200 DEG C；
Reaction pressure: normal pressure~2MPa；
Liquid hourly space velocity (LHSV): 1~50h-1。
Flyash is mixed and is roasted with binder for the poor problem of catalyst system stability in the prior art by the present invention
Burning obtains flyash catalyst, and the flyash catalyst is used for the processing of organic wastewater microwave catalysis oxidation.Using the present invention
Flyash catalyst substitute existing active carbon and activated alumina catalyst system, improve organic wastewater microwave catalysis system
Stability.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.Below in conjunction with embodiment, the present invention will be described in detail.
In order to improve the stability of organic wastewater microwave catalysis system, according to an aspect of the invention, there is provided a kind of
The preparation method of flyash catalyst, method includes the following steps: will include that flyash is mixed and roasted with the raw material of binder
It burns, obtains flyash catalyst.The present invention is innovatively proposed using flyash as microwave catalysis oxidation processing organic wastewater
Catalyst body obtains the caltalyst that intensity is good, catalytic stability is high by mixing and roasting flyash with binder
System.It is a discovery of the invention that the flyash catalyst prepared using the above method, can solve to use Al2O3And the porous materials such as active carbon
The problems such as poor in microwave reaction condition stability inferior, longtime running catalyst activity component is lost, catalytic efficiency decline.
Also, method of the invention realizes the resource utilization of flyash simultaneously.Coal-burning power plant is every to be discharged every year
Hundred million tons of flyash not only need to occupy a large amount of lands used and are stored, but also since fugitive dust and harmful element are leached to ecological around
Environment causes to seriously endanger.The present invention realizes the resource utilization of flyash, solves the environment of flyash to a certain extent
Harm problem.
Method of the invention needs first to mix flyash with binder.The weight ratio of flyash and binder can root
It is adjusted according to needs.Preferably, the weight ratio of flyash and binder is 1~10:1.In the proportional region, it can be ensured that
The better mouldability of flyash catalyst, and also can ensure that it is used for the preferable of microwave catalysis oxidation processing organic wastewater
Catalytic effect.
After mixing flyash with binder, they are roasted, the temperature of roasting is preferably 300~900 DEG C, roasting
The time of burning is preferably 2~24 hours.After roasting the above-mentioned time under above-mentioned temperature range, high-intensitive, high stable can be obtained
The flyash catalyst of property.
Before above-mentioned calcination steps, method of the invention further includes carrying out at molding to flyash and binder raw material
Reason, preferably carries out kneaded and formed.Since there may be certain moisture in binder, it is preferable that can be to raw material after molding
It is dried, the temperature of drying process is preferably 80~120 DEG C, and the time is preferably 4~12 hours.
In the present invention, flyash refers to the primary solids waste of the discharges such as coal-burning power plant, it includes main oxides
Are as follows: SiO2、Al2O3、Fe2O3Deng.Due to the presence of these metal oxides in flyash, allow to using flyash as catalysis
Agent main body, the microwave catalysis oxidation for organic wastewater are handled.
Preferably, the flying dust or recirculating fluidized bed that the flyash that the present invention uses can generate for coal-burning power plant's pulverized-coal fired boiler
The Desulphurization that boiler generates.
Particularly, in the present invention it is possible to use silica solution, Aluminum sol and any one or more of work of methylcellulose
For binder.These binders have many advantages, such as that caking property is high, stability is high, suitable for prepare present invention contemplates that flyash urge
Agent.
According to another aspect of the present invention, a kind of flyash catalyst is provided, the flyash catalyst is by the present invention
The above method be prepared.Flyash catalyst strength of the invention is good, catalytic stability is high, can solve to use Al2O3And it is living
The porous materials such as property charcoal are poor in microwave reaction condition stability inferior, the loss of active component of longtime running catalyst, catalytic efficiency
The problems such as decline.
According to a further aspect of the invention, a kind of processing method of organic wastewater is provided, which includes to having
Machine waste water carries out microwave catalysis oxidation processing, and the catalyst of microwave catalysis oxidation processing is by above-mentioned preparation method system of the invention
It is standby to obtain.Method for processing organic wastewater of the invention solves the prior art due to using above-mentioned flyash catalyst system
The problems such as middle catalyst stability is poor, and longtime running catalytic efficiency declines.Also, organic waste is handled using method of the invention
Water, COD removal rate is up to 60% or more, preferably up to 70% or more, and treated, and waste water is easy to biological oxidation processing.
Method of the invention is particularly suitable for handle the organic wastewater of high concentration, specifically, the high concentrated organic wastewater
COD value is 3000~100000.
Preferably, microwave catalysis oxidation processing includes following process conditions:
Microwave frequency: 400~3000MHz, preferably 915MHz or 2450MHz；
Power: 100~5000W, preferably 400~1000W；
Reaction temperature: room temperature~200 DEG C；
Reaction pressure: normal pressure~2MPa；
Liquid hourly space velocity (LHSV) (LHSV): 1~50h-1。
Liquid hourly space velocity (LHSV) refers to the volume flow (m of the organic wastewater as raw material3.h-1)/catalyst volume (m3)
Under above-mentioned process conditions, the efficient process to organic wastewater can be realized.
In addition, in microwave catalysis oxidation processing, it is preferred to use oxygen or air are as oxidant.
Beneficial effects of the present invention are further illustrated below in conjunction with embodiment.
Embodiment 1
Catalyst preparation: taking 100 grams of flyash, and 20 grams of silica solution is added, 4 hours dry at 80 DEG C after kneaded and formed,
In 300 DEG C of roastings, 2 hours obtained catalyst.
Microwave catalysis oxidation processing: 20 grams of catalyst are added in microwave catalysis reactor, by CODCr=13580mg/L's
High concentrated organic wastewater is pumped into, and treatment conditions are as follows: microwave frequency: 915MHz；Power: 800W；Reaction temperature: room temperature；Reaction
Pressure: normal pressure；Liquid hourly space velocity (LHSV) (LHSV): 1h-1；Oxidant: oxygen.
Processing result: processed waste water CODCr=3938mg/L, COD removal rate 71%.This waste water is further passed through life
Change method processing unit, processed waste water CODCr=72mg/L.
After microwave catalysis oxidation reaction is carried out continuously 100 hours, COD removal rate changes less substantially, maintains 68% left side
The right side, the mechanical strength that catalyst is split out after reaction, which has no, to be substantially reduced.
Embodiment 2
Catalyst preparation: taking 100 grams of flyash, and 15 grams of Aluminum sol is added, small in 120 DEG C of dryings 12 after kneaded and formed
When, in 900 DEG C of roastings, 24 hours obtained catalyst.
Microwave catalysis oxidation processing: as described in Example 1.
Processing result: processed waste water CODCr=2716mg/L, COD removal rate 80%.This waste water is further passed through life
Change method processing unit, processed waste water CODCr=38mg/L.
After microwave catalysis oxidation reaction is carried out continuously 100 hours, COD removal rate changes less substantially, maintains 78% left side
The right side, the mechanical strength that catalyst is split out after reaction, which has no, to be substantially reduced.
Embodiment 3
Catalyst preparation: taking 100 grams of flyash, is added 10 grams of methylcellulose, it is kneaded and formed after in 100 DEG C of dryings
6 hours, in 900 DEG C of roastings, 4 hours obtained catalyst.
Microwave catalysis oxidation processing: 20 grams of catalyst are added in microwave catalysis reactor, by CODCr=13580mg/L's
High concentrated organic wastewater is pumped into, and treatment conditions are as follows: microwave frequency: 2450MHz；Power: 1000W；Reaction temperature: 100 DEG C；Instead
Answer pressure: 2MPa；Liquid hourly space velocity (LHSV) (LHSV): 20h-1；Oxidant: oxygen.
Processing result: processed waste water CODCr=2988mg/L, COD removal rate 78%.This waste water is further passed through life
Change method processing unit, processed waste water CODCr=41mg/L.
After microwave catalysis oxidation reaction is carried out continuously 100 hours, COD removal rate changes less substantially, maintains 75% left side
The right side, the mechanical strength that catalyst is split out after reaction, which has no, to be substantially reduced.
Embodiment 4
Catalyst preparation: taking 100 grams of flyash, and 100 grams of silica solution are added, small in 100 DEG C of dryings 6 after kneaded and formed
When, in 750 DEG C of roastings, 6 hours obtained catalyst.
Microwave catalysis oxidation processing: as described in Example 3.
Processing result: processed waste water CODCr=2580mg/L, COD removal rate 81%.This waste water is further passed through life
Change method processing unit, processed waste water CODCr=36mg/L.
After microwave catalysis oxidation reaction is carried out continuously 100 hours, COD removal rate changes less substantially, maintains 76% left side
The right side, the mechanical strength that catalyst is split out after reaction, which has no, to be substantially reduced.
Embodiment 5
Catalyst preparation: as described in Example 1, the difference is that: 8 grams of silica solution is added.
Microwave catalysis oxidation processing: as described in Example 1.
Processing result: processed waste water CODCr=4074mg/L, COD removal rate 70%.This waste water is further passed through life
Change method processing unit, processed waste water CODCr=74mg/L.
After microwave catalysis oxidation reaction is carried out continuously 100 hours, COD removal rate changes less substantially, maintains 65% left side
The right side, the mechanical strength that catalyst is split out after reaction, which has no, to be substantially reduced.
Embodiment 6
Catalyst preparation: as described in Example 1, the difference is that: 105 grams of silica solution is added.
Microwave catalysis oxidation processing: as described in Example 1.
Processing result: processed waste water CODCr=4346mg/L, COD removal rate 68%.This waste water is further passed through life
Change method processing unit, processed waste water CODCr=78mg/L.
After microwave catalysis oxidation reaction is carried out continuously 100 hours, COD removal rate changes less substantially, maintains 60% left side
The right side, the mechanical strength that catalyst is split out after reaction, which has no, to be substantially reduced.
Comparative examples 1
20 grams of absorbent charcoal carriers are taken, 10%Mn (NO is immersed3)2It is 6 hours dry at 100 DEG C after aqueous solution 12 hours, 550
DEG C roasting 6 hours after be made catalyst, by this catalyst be placed in microwave catalysis reactor in, waste water to be processed and treatment conditions are same
Embodiment 1, initial COD removal rate 83%, after continuous operation 100 hours, COD removal rate drops to 50% hereinafter, giving up after processing
There are a large amount of black powders in water, the post catalyst reaction intensity split out is decreased obviously, and catalyst weight is substantially reduced.
Comparative examples 2
20 grams of active aluminum oxide carriers are taken, 10%Mn (NO is immersed3)2And Ce (NO3)3After aqueous solution 12 hours, at 100 DEG C
It is 6 hours dry, catalyst is made after roasting 6 hours at 550 DEG C, this catalyst is placed in microwave catalysis reactor, it is to be processed
Waste water and treatment conditions are with embodiment 1, and initial COD removal rate 85%, after continuous operation 100 hours, COD removal rate drops to
70% hereinafter, the post catalyst reaction intensity split out is decreased obviously, and catalyst activity component proportion is substantially reduced.
As can be seen from the above-described embodiment, the flyash of microwave catalysis oxidation of the invention processing high concentrated organic wastewater is urged
Agent has the advantages that
1. the flyash catalytic mechanical intensity of microwave catalysis oxidation processing high concentrated organic wastewater of the invention is good, stablize
Property it is high, the service life is long.
2. use catalyst microwave oxidation treated high concentration organic wastewater of the present invention, COD removal rate up to 60% or more,
In the case that flyash and weight of binder ratio are 1~10:1, COD removal rate is easy to further even up to 70% or more
The processing of ground biological oxidation.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of flyash catalyst, which is characterized in that the described method comprises the following steps:
It will include that flyash is mixed and roasted with the raw material of binder, obtain the flyash catalyst.
2. preparation method according to claim 1, which is characterized in that the weight ratio of the flyash and the binder is
1~10:1.
3. preparation method according to claim 1, which is characterized in that the temperature of the roasting is 300~900 DEG C, described
The time of roasting is 2~24 hours.
4. preparation method described in any one of claim 1 to 3, which is characterized in that before the roasting the step of,
The method also includes carrying out forming processes to the raw material, the preferably described forming processes are kneaded and formed；To institute after molding
Raw material to be stated to be dried, the temperature of the preferably described drying process is 80~120 DEG C, the time of the drying process is 4~
12 hours.
5. preparation method described in any one of claim 1 to 3, which is characterized in that the flyash at least contain with
Lower ingredient: SiO2、Al2O3And Fe2O3。
6. preparation method described in any one of claim 1 to 3, which is characterized in that the binder is silica solution, aluminium
Colloidal sol and methylcellulose are any one or more of.
7. a kind of flyash catalyst, which is characterized in that the flyash catalyst is as described in any one of claim 1~6
Preparation method be prepared.
8. a kind of processing method of organic wastewater the treating method comprises and carry out at microwave catalysis oxidation to the organic wastewater
Reason, which is characterized in that the catalyst of the microwave catalysis oxidation processing is by preparation side according to any one of claims 1 to 6
Method is prepared.
9. processing method according to claim 8, which is characterized in that the COD value of the organic wastewater be 3000~
100000。
10. processing method according to claim 8 or claim 9, which is characterized in that the microwave catalysis oxidation processing includes following
Process conditions:
Microwave frequency: 400~3000MHz；
Power: 100~5000W；
Reaction temperature: room temperature~200 DEG C；
Reaction pressure: normal pressure~2MPa；
Liquid hourly space velocity (LHSV): 1~50h-1。
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Application publication date: 20190820 |