CN107096517A - Nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere - Google Patents
Nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere Download PDFInfo
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- CN107096517A CN107096517A CN201710329309.9A CN201710329309A CN107096517A CN 107096517 A CN107096517 A CN 107096517A CN 201710329309 A CN201710329309 A CN 201710329309A CN 107096517 A CN107096517 A CN 107096517A
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- flyash
- micro wave
- encloses
- carbon dioxide
- regeneration method
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3441—Regeneration or reactivation by electric current, ultrasound or irradiation, e.g. electromagnetic radiation such as X-rays, UV, light, microwaves
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The invention discloses the micro wave regeneration method that nitrogen dioxide and carbon dioxide mix atmosphere enclose lower flyash.Flyash KMnO of the invention by adsorption saturation4Solution is pre-processed, and is subsequently placed in microwave equipment, and flyash is in state of disturbance under mechanical stirring, is passed through a certain amount of NO2、CO2Gaseous mixture, control microwave power and recovery time, carry out microwave radiation regeneration.Stop microwave heating, in N2、CO、H2Gaseous mixture atmosphere under flyash is cooled to room temperature, obtain regenerate flyash.The present invention takes full advantage of the advantage that microwave heating is efficient, quick, save, and reproduction speed is fast, the low, flyash that consumes energy is recycled often, with good environment benefits and economic gains.
Description
Technical field
The present invention relates to a kind of technique of microwave flyash regeneration, more particularly to one kind fine coal is carried out using microwave technology
The technique of ash regeneration, belongs to field of environmental engineering.
Background technology
Flyash is a kind of attritive powder with pozzolanic activity, and Main chemical component is Al2O3、Fe2O3、SiO2Deng.
Fly ash grain physical organization is porous, and specific surface area is larger, with higher adsorption activity, and cheap, wide material sources.Powder
Coal ash is gradually applied as a kind of sorbing material in water process, oil processing field.But the flyash hole after adsorption saturation
Gap structure is adsorbed matter and blocked, and loses adsorption capacity.And after absorption harmful substance, its own turns into a kind of venomous injurant
Matter.The direct discarding of saturation absorption flyash can cause environmental pollution, by regeneration can allow suction its be recycled for multiple times, at reduction
Manage cost, reduce the generation of waste residue.Therefore, regeneration is a kind of good processing mode.
The regeneration of sorbing material refers to, with physics, chemistry or biological method, the adsorbate on sorbing material surface be departed from
Or decompose, recover its absorption property.Regneration of adsorbent material method has hot recycling, solvent reclamation, Photocatalytic Regeneration, electrochemistry again
Life, the regeneration of wet air regeneration method, supercritical fluid etc..
In various renovation process, hot recycling method is the method for most study, technology maturation the most.But hot recycling method consumes energy
Big, the recyclable number of times of high, sorbing material thermal losses is few, and does not meet environmental protection, the requirement of energy-conservation.It is therefore desirable to have other more preferable
Renovation process.
Microwave reclaiming method substantially falls within hot recycling, but its thermal conduction mechanism with traditional hot recycling is variant.The latter
Heat transfer be " from outside to inside " that the former is overall heating, heat results from internal rather than from external heat source.It is this unique
Mode of heating cause microwave firing rate faster, with selective, energy-efficient.Micro wave regeneration also have the time it is short, consume energy it is low,
The advantages of small to sorbing material damage, the concern of numerous researchers has been obtained.
The renovation process that existing microwave heating regeneration technology is introduced, is only limitted to activated carbon, silica gel etc. several limited
Sorbing material.Such as patent ZL201410028853.6, CN201510939699.2 describes the micro wave regeneration of activated carbon,
ZL201520318302.3 describes the micro wave regeneration of silica gel.
Therefore, it is necessary to be extended to micro wave regeneration technology on flyash using scope, a kind of speed of design research and development is fast,
Energy consumption is low, non-secondary pollution, the high regeneration treating method of flyash quality after simple to operate, regeneration.
The content of the invention
It is an object of the invention to provide the micro wave regeneration side that nitrogen dioxide and carbon dioxide mix atmosphere enclose lower flyash
Method.The present invention is in the micro wave regeneration of flyash, by NO2As reaction gas, flyash regeneration efficiency and reproduction quality are improved.
The present invention is realized by following technical proposal：Nitrogen dioxide encloses the microwave of lower flyash with carbon dioxide mix atmosphere
Renovation process, by following each step：
A, the flyash of adsorption saturation is placed in KMnO4Handled in solution, then by the first alkali cleaning of treated flyash, wash again
To neutrality.
B, by KMnO4Flyash after solution processing is placed in microwave equipment, is started mechanical agitation, is passed through NO2、CO2Mixing
Gas, controls microwave power, and flyash is heated using microwave radiation.
C, stopping microwave equipment, in N2、CO、H2Flyash is cooled down under gaseous mixture atmosphere, stored for future use.
The beneficial effects of the present invention are：
（1）Micro wave regeneration technology is applied on Powder ash adsorption material by the present invention, expands the model of micro wave regeneration sorbing material
Enclose.Flyash is realized waste resource and comprehensively utilized again by micro wave regeneration, and meeting recycling economy will with environment-friendly
Ask；
（2）The present invention uses NO in the micro wave regeneration of flyash2As reaction gas, improve flyash micro wave regeneration efficiency and
Quality.Flyash micro wave regeneration efficiency for water process can improve the % of 4.7 % ~ 10.7；Flyash for waste oil disposal is micro-
Ripple regeneration efficiency can improve the % of 6.3 % ~ 10.2.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
The present invention is described further with reference to embodiment.
The present embodiment 1, comprises the following steps：
The first step, the screening of original state flyash.
Gradation sizing is carried out to the flyash for being derived from certain power plant, large granular impurity is removed, chooses the mm of particle diameter 0.03 ~ 0.05
Flyash.The flyash of selection is embathed with deionized water, until it is transparent to embathe water colorless.The flyash for embathing clean is put into
60 DEG C of baking oven dries 6 h, obtains fresh coal fly ash.
Second step, fresh coal fly ash is to the absorption of methylene blue waste water and producing for waste fly ash.
100 g fresh coal fly ashs are taken in 1000 ml conical flasks, according to 0.2 g/ml dosage, 500 ml are poured into sub-
Methyl blue solution.1 h is adsorbed under 40 DEG C of water-baths, the r/min of magnetic agitation 300.Filtered using double-layer filter paper, filter residue spend from
Sub- water is rinsed until clean repeatedly, and the baking oven for being put into 60 DEG C dries 6 h, obtains waste fly ash.Filtrate is taken, is determined at 664 nm light
Its absorbance, methylene blue solution concentration is calculated according to standard curve, calculates the absorption of the clearance and flyash of methylene blue
Capacity.
The adsorption capacity calculation formula of flyash is：, in formula,c 0 For methylene blue initial concentration before absorption
（mg/L）；cFor methylene blue concentration after absorption（Mg/L）；q 1 For unit quality Powder ash adsorption amount（Mg/g）；m For flyash
Dry weight（g）；VFor liquor capacity（L）.
3rd step, the pretreatment of waste fly ash.
Take 100 g to adsorb the flyash after methylene blue waste water, be that mass fraction is that 8 %, pH are 3 with 500 ml concentration
KMnO4Solution soaks 60 min.By KMnO4The treated flyash of solution is embathed with 600 ml concentration for 2.5 mol/L NaOH
20 min, then clean flyash to washing lotion in neutrality with distilled water.
4th step, waste fly ash first time micro wave regeneration.
Take two parts of KMnO of A, B4Solution is treated, and moisture content is 25 % flyash, is respectively placed in microwave equipment and is regenerated.
A regeneration condition is：The g of flyash quality 50, starts mechanical agitation, regulation mixing speed 400 r/min.It is passed through:=1:3 mixed gas, adjusts the m/s of flow velocity 1.5,3 min is kept, with the air in the system of driving away.Keep mixed
Close gas to be passed through and flow velocity, start microwave equipment, adjust the W of microwave power 800, radiate 4 min.Stop microwave equipment, change and be passed through
Flow velocity is 1.5 m/s N2, CO and H2Gaseous mixture, wherein:=1:3,:=1:4.Continue gaseous mixture to be passed through
Until flyash is cooled to room temperature, obtain regenerating flyash.
B regeneration condition is：The g of flyash quality 50, starts mechanical agitation, regulation mixing speed 400 r/min.It is passed through:=1:12 mixed gas, adjusts the m/s of flow velocity 1.5,3 min is kept, with the air in the system of driving away.Keep mixed
Close gas to be passed through and flow velocity, start microwave equipment, adjust the W of microwave power 800, radiate 4 min.Stop microwave equipment, change and be passed through
Flow velocity is 1.5 m/s N2, CO and H2Gaseous mixture, wherein:=1:3,:=1:4.Continue gaseous mixture to be passed through
Until flyash is cooled to room temperature, obtain regenerating flyash.
5th step, absorption of the regeneration flyash to methylene blue waste water.
Respectively take 50 g to regenerate flyash in conical flask in A, B, according to 0.2 g/ml dosage, pour into 250 ml sub-
Methyl blue solution.1 h is adsorbed under 40 DEG C of water-baths, the r/min of magnetic agitation 300.Filtrate is taken using double-layer filter paper, in 664 nm
Its absorbance is determined at light, methylene blue solution concentration is calculated according to standard curve, the adsorption capacity of flyash is calculated, is designated asq 2 。Calculate first time micro wave regeneration efficiency：
The first time micro wave regeneration efficiency of flyash is,。
6th step, the multiple absorption regeneration of flyash.
The flyash after the absorption of the 5th step is taken, third and fourth step operation is carried out, calculates second of micro wave regeneration efficiency.Weight
Multiple aforesaid operations, obtain A, B the 3rd, the 4th micro wave regeneration efficiency, are shown in Table 1.
The micro wave regeneration efficiency of table 1
As shown in Table 1, B groups flyash regeneration efficiency illustrates that method of the invention can improve powder higher than the % of the % of A groups 4.7 ~ 10.7
The regeneration efficiency and reproduction quality of coal ash.
The present embodiment 2, comprises the following steps：
The first step, the screening of flyash and the pretreatment of waste oil.
Gradation sizing is carried out to the flyash for being derived from certain power plant, large granular impurity is removed, chooses the mm of particle diameter 0.03 ~ 0.05
Flyash.The flyash of selection is embathed with deionized water, until it is transparent to embathe water colorless.The flyash for embathing clean is put into
60 DEG C of baking oven dries 6 h, obtains fresh coal fly ash.The useless machinery oil for being derived from certain factory is filtered off using 400 ~ 800 mesh mesh screens bad
Change the larger suspended impurity in machinery oil.Finally the waste oil after removal of impurities is placed in centrifugal separator, gone by centrifuging
Except the residual impurity in waste oil, the mgKOH/g of acid number 0.823 is obtained（GB/T264）Machinery oil.
Second step, fresh coal fly ash is to the absorption of acid number in waste oil and producing for waste fly ash.
100 g fresh coal fly ashs are taken in conical flask, according to 0.1 g/ml dosage, the useless machinery oil of 1 L are poured into.90
55 min are adsorbed under DEG C oil bath, the r/min of magnetic agitation 300.Flyash, fluid are separated with suction filtration machine.The flyash that sub-argument goes out
Petroleum ether extracted many times are used, flyash surface fluid is removed, is then placed in baking oven, 12 h are dried at 70 DEG C, useless fine coal is obtained
Ash.The fluid isolated is centrifuged under 10000 r/min centrifuge, takes the upper strata fluid after centrifugation with 905 titrando types
Potentiometric titrimeter determines its acid number, calculates the clearance of acid number and the adsorption capacity of flyash.
The acid number adsorption capacity calculation formula of flyash is：, in formula,c 0 At the beginning of machinery oil acid number before absorption
Beginning concentration（mgKOH/g）；cFor machinery oil acid number concentration after absorption（mgKOH/g）；q 1 For unit quality Powder ash adsorption amount（Mg/
g）；mFor flyash dry weight（g）；V For fluid volume（L）.
3rd step, the pretreatment of waste fly ash.
The flyash after 100 g adsorption treatment waste oil is taken, is that mass fraction is that 8 %, pH are 3 with 500 ml concentration
KMnO4Solution soaks 60 min.By KMnO4The treated flyash of solution is embathed with 600 ml concentration for 2.5 mol/L NaOH
20 min, then clean flyash to washing lotion in neutrality with distilled water.
4th step, waste fly ash first time micro wave regeneration.
Take two parts of KMnO of A, B4Solution is treated, and moisture content is 25 % flyash, is respectively placed in microwave equipment and is regenerated.
A regeneration condition is：The g of flyash quality 50, starts mechanical agitation, regulation mixing speed 400 r/min.It is passed through:=1:3 mixed gas, adjusts the m/s of flow velocity 1.5,3 min is kept, with the air in the system of driving away.Keep mixed
Close gas to be passed through and flow velocity, start microwave equipment, adjust the W of microwave power 800, radiate 4 min.Stop microwave equipment, change and be passed through
Flow velocity is 1.5 m/s N2, CO and H2Gaseous mixture, wherein:=1:3,:=1:4.Continue gaseous mixture to be passed through
Until flyash is cooled to room temperature, obtain regenerating flyash.
B regeneration condition is：The g of flyash quality 50, starts mechanical agitation, regulation mixing speed 400 r/min.It is passed through:=1:12 mixed gas, adjusts the m/s of flow velocity 1.5,3 min is kept, with the air in the system of driving away.Keep mixed
Close gas to be passed through and flow velocity, start microwave equipment, adjust the W of microwave power 800, radiate 4 min.Stop microwave equipment, change and be passed through
Flow velocity is 1.5 m/s N2, CO and H2Gaseous mixture, wherein:=1:3,:=1:4.Continue gaseous mixture to be passed through
Until flyash is cooled to room temperature, obtain regenerating flyash.
5th step, adsorption treatment of the regeneration flyash to the machinery oil that gives up.
Respectively take 50 g to regenerate flyash in conical flask in A, B, according to 0.1 g/ml dosage, pour into 50 ml and give up
Machinery oil.55 min are adsorbed under 90 DEG C of oil baths, the r/min of magnetic agitation 450.Flyash, fluid are separated with suction filtration machine.Point
The fluid separated out is centrifuged under 10000 r/min centrifuge, takes the upper strata fluid after centrifugation with 905 titrando type current potentials
Titrator determines its acid number, calculates flyash to acid number adsorption capacityq 2.Calculate first time micro wave regeneration efficiency：
The first time micro wave regeneration efficiency of flyash is,。
6th step, the multiple absorption regeneration of flyash.
The flyash after the absorption of the 5th step is taken, third and fourth step operation is carried out, calculates second of micro wave regeneration efficiency.Weight
Multiple aforesaid operations, obtain A, B the 3rd, the 4th micro wave regeneration efficiency, are shown in Table 2.
The micro wave regeneration efficiency of table 2
As shown in Table 2, B groups flyash regeneration efficiency illustrates that method of the invention can improve powder higher than the % of the % of A groups 6.3 ~ 10.2
The regeneration efficiency and reproduction quality of coal ash.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to compared with
The present invention is described in detail good embodiment, it will be understood by those within the art that, can be to skill of the invention
Art scheme is modified or equivalent substitution, and without departing from the objective and scope of technical solution of the present invention, it all should cover at this
Among the right of invention.
Claims (9)
1. nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere, it is characterised in that methods described
Comprise the following steps：
A, the flyash of adsorption saturation is placed in KMnO4Handled in solution, then by the first alkali cleaning of treated flyash, wash again
To neutrality；
B, by KMnO4Flyash after solution processing is placed in microwave equipment, is started mechanical agitation, is passed through NO2、CO2Gaseous mixture,
Microwave power is controlled, flyash is heated using microwave radiation；
C, stopping microwave equipment, in N2、CO、H2Gaseous mixture atmosphere under flyash is cooled down, store for future use.
2. nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere according to claim 1, its
It is characterised by, the KMnO that flyash is pre-processed is used for described in step A4Liquid quality fraction is the % of 5 % ~ 14, and pH value of solution is 2 ~ 4,
Flyash quality and KMnO4Liquor capacity ratio is 1:3~1:7, the min of processing time 50 ~ 90.
3. nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere according to claim 1, its
It is characterised by, the alkali wash water described in step A for flyash is NaOH or KOH solution, concentration is 1.5 ~ 3.2 mol/L, fine coal
Grey quality is 1 with alkali wash water volume ratio:4~1:8, the min of alkali cleaning time 10 ~ 30.
4. nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere according to claim 1, its
It is characterised by, the moisture content of the flyash described in step B is the % of 18 % ~ 34.
5. nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere according to claim 1, its
It is characterised by, the r/min of mechanical agitation speed 200 ~ 500 described in step B.
6. nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere according to claim 1, its
It is characterised by, NO in the gaseous mixture being passed through described in step B2With CO2Volume ratio, i.e.,:=1:8~1:19。
7. nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere according to claim 1, its
It is characterised by, the mixed gas flow velocity being passed through described in step B is 0.015 ~ 0.035 m/sg with flyash quality ratio-1。
8. nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere according to claim 1, its
It is characterised by, microwave power described in step B is 10 ~ 30 W/g with flyash quality ratio, microwave irradiation time is 2 ~ 6 min.
9. nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere according to claim 1, its
It is characterised by, CO and H in gaseous mixture described in step C2Volume ratio, i.e.,:=1:1~1:5, CO, H2Volume sum and N2Body
Product ratio, i.e.,:=1:3~1:7, mixed gas flow velocity is 0.01 ~ 0.03 m/sg with flyash quality ratio-1。
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Citations (3)
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2017
- 2017-05-11 CN CN201710329309.9A patent/CN107096517A/en active Pending
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|---|---|---|---|---|
| CN102616778A (en) * | 2012-04-06 | 2012-08-01 | 昆明理工大学 | Method for preparing mesoporous activated carbon by regenerating waste coal-based activated carbon through microwave heating |
| CN103447015A (en) * | 2013-07-24 | 2013-12-18 | 浙江工业大学 | Desorption and regeneration method for organic matter adsorbent |
| CN106268626A (en) * | 2015-06-12 | 2017-01-04 | 南京工业大学 | A kind of renovation process of magnetic diatomite adsorbant |
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