CN107486150A - A kind of preparation method for being used to cooperate with the activated carbon of microwave degradation coking chemical waste water - Google Patents
A kind of preparation method for being used to cooperate with the activated carbon of microwave degradation coking chemical waste water Download PDFInfo
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- CN107486150A CN107486150A CN201710718102.0A CN201710718102A CN107486150A CN 107486150 A CN107486150 A CN 107486150A CN 201710718102 A CN201710718102 A CN 201710718102A CN 107486150 A CN107486150 A CN 107486150A
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0222—Compounds of Mn, Re
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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Abstract
The invention discloses a kind of preparation method for being used to cooperate with the activated carbon of microwave degradation coking chemical waste water, this method is by clay, Fe3O4Powder, wooden powder absorbent charcoal, copper powder and manganese powder add starch, Regularization activated carbon is made by mixing, shaking the processes such as ball, drying and firing, the Regularization activated carbon and coking chemical waste water are placed in microwave dissolver and cleared up, after resolution reaction cooling terminates, micro-wave diminishing pot is taken out, by the coking chemical waste water filter centrifugation after processing.Ammonia nitrogen (the NH in coking chemical waste water can be made3N) and COD (COD) can reach 88.4% -92.54%, 85% -98.14% except rate.
Description
Technical field
The invention belongs to field of environment engineering, more particularly to a kind of rule for being used to cooperate with organic matter in microwave degradation coking chemical waste water
Integralization absorbent charcoal material and preparation method thereof.
Background technology
China is the big country of world's coke production flow control one.The coking industry of China is developed rapidly since two thousand,
Coal chemical enterprise caused pollution problem when producing coal also constantly shows therewith.Coking industry is all severe dirt all the time
The enterprise of dye, the toxic industrial waste water of its difficult degradation formed, can bring serious harm to ecological environment and human health.It is burnt
It is coal industrial wastewater for being formed during high-temperature retorting and during gas purification, byproduct recovery etc. to change waste water, wherein
Contain tens kinds of high concentration organic contaminants such as ammonia nitrogen, phenol, cyanogen, benzene DDGS, polycyclic aromatic hydrocarbon, these organic pollution colourities
Height, toxicity is big, and property is stable, so that it is difficult to handled with biological degradation method, and some organic pollutants have the characteristics of carcinogenic,
So Treatment of Wastewater in Coking is great environmental issue urgently to be resolved hurrily.
At present, method of chemical treatment, the Fenton such as the microorganism treatment such as activated sludge technology, ozone Oxidation Treatment technology
The biologies such as reagent technique-chemical combined method is widely used in removing the organic pollution in coking chemical waste water, but these methods
Complex operation, the reaction time is long, treatment effeciency is low and has generation secondary pollution problems.Microwave-activated carbon treatment technology is one
Kind is with economic, efficient, New Wastewater Treatment Technology art with broad prospects for development.
The content of the invention
It is an object of the invention to provide a kind of preparation method for being used to cooperate with the activated carbon of microwave degradation coking chemical waste water, make
With absorbent charcoal material produced by the present invention, and microwave technology Treatment of Wastewater in Coking is cooperateed with, utilize microwave to make the modified of activated carbon
With the synergy with microwave, activated carbon, the organic pollution removed in coking chemical waste water rapidly and efficiently.On the one hand microwave is utilized
Hot spot-effect and non-thermal point effect, microwave energy is changed into heat energy, reaction physically or chemically not only occurs between inducing molecule,
The activation energy of reaction can also be reduced.On the other hand, under the radiation of microwave, system temperature raises rapidly, so that activated carbon duct
For the organic matter of middle absorption coking chemical waste water due to being decomposed in vaporization at high temperature or charing, final mineralising produces CO2, the gas weight such as vapor
New pore-creating, i.e. regenerating active carbon.
Compared to other treatment technologies, microwave-activated carbon technology has ageing, globality, selectivity, high efficiency, work
Property charcoal it is renewable the advantages that, therefore microwave-activated carbon wave technology turn into recent years Technologies of Coke Plant Wastewater Treatment innovation focus.
Microwave-activated carbon treatment effect is not the simple addition of microwave treatment effect and activated carbon treatment effect.
Activated carbon has stronger absorbability to microwave, the characteristics of easily absorbing microwave along with some magnetic oxides, activated carbon surface
The metal or metal oxide of attachment can be formed many " focuses " under the irradiation of microwave, and the organic molecule in coking chemical waste water exists
In the presence of warm-up movement, adsorb in activated carbon surface, with the effect of microwave radiation, work of the organic matter in 1000 DEG C or so temperature
On property center, by rapid pyrolitic oxidation.
The present invention prepares novel absorbent charcoal solid powder using optimum ratio, used with pellet rocker shaken into by the method for adding water it is straight
Footpath is 5mm-10mm activated carbon, after drying in an oven, the activated carbon of Regularization is made of Muffle furnace roasting, is referred to as the present invention
Activated carbon.
The present invention comprises the following steps:
Step A:After clay is the higher clay crushing of viscosity, obtained after 0.075mm sieves, i.e. clay particle
The small 0.075mm of diameter;Wooden powder absorbent charcoal is acidified with hydrochloric acid, after distilled water flushing to neutrality, is placed in kept dry in baking oven
It is standby;
Step B:According to mass ratio, clay, Fe made from step A are weighed respectively3O4Powder, wooden powder absorbent charcoal, copper powder and
Manganese powder;All solids powder is placed in same container and uniformly mixed;
Step C:Take starch to add in clay to be well mixed, shake into a diameter of 0.5mm -1mm's by the way of water dropwise
Spheroid, referred to as activated carbon core, the activated carbon core is placed in drying for standby in baking oven;
Step D:By obtained activated charcoal solid powder and activated carbon core and mixing in step B and step C, shaken with pellet rocker
The initial activity charcoal of Regularization is made, after being dried in baking oven, Muffle furnace burns till Regularization activated carbon.
In above-mentioned steps A, the specific method of wooden powder absorbent charcoal activation is:Wooden powder absorbent charcoal is placed in 0.5mol/
Half an hour is soaked in L -1.0mol/L hydrochloric acid, is neutral with distilled water filtration and washing to pH, is done in 50 DEG C -80 DEG C of baking oven
Dry 1h -2h.
In above-mentioned steps B, clay, Fe3O4Powder, wooden powder absorbent charcoal, copper powder, manganese powder are 8 according to mass ratio:21:8:
4:7 weigh, and are well mixed standby.
In above-mentioned steps C, starch quality is with clay mass ratio according to 1:3–1:4 are weighed, and diameter is shaken into after well mixed
For 0.5mm -1mm activated carbon core, 1h -2h are dried in 50 DEG C -80 DEG C of baking oven.
In above-mentioned steps D, obtained activated charcoal solid powder in step B and step C and activated carbon core are mixed, with shaking
Grain machine shakes the initial activity charcoal that Regularization is made, and after drying 1h -2h in 50 DEG C of -80 DEG C of baking ovens, then takes out and is covered with quartz sand
Cover on its surface, 2-3h are burnt under conditions of 300 DEG C-400 DEG C of Muffle furnace into Regularization activated carbon.
The mass fraction that Regularization activated carbon produced by the present invention contains clay is 15% -30%, wooden powder absorbent charcoal matter
Amount fraction is 10% -15%, Fe3O4Mass fraction is 40% -50%, and copper powder mass fraction is 15% -20%, manganese powder quality point
Number is 5% -10%.
The method handled using Regularization activated carbon coking chemical waste water, this method are:
Regularization activated carbon and coking chemical waste water are placed in microwave dissolver and cleared up, to the end of cooling is reacted in resolution
Afterwards, micro-wave diminishing pot is taken out, by the coking chemical waste water filter centrifugation after processing.Make the ammonia nitrogen (NH in coking chemical waste water3- N) and chemistry
Oxygen demand (COD) can reach 88.4% -92.54%, 85% -98.14% except rate.
The concentration of the coking chemical waste water is 150mg/L-200mg/L, and the initial pH value of coking chemical waste water is 8-10, and Regularization is lived
Property carbonaceous amount and coking chemical waste water volume ratio be 1:20–1:25;Microwave power is 400W -600W, exposure time be 5min -
8min。
Coking chemical waste water after the filtering is centrifuged under conditions of rotating speed is 300r/min -500r/min.
Beneficial effects of the present invention:
1st, Regularization activated carbon produced by the present invention, the ammonia nitrogen (NH in coking chemical waste water can be made3- N) and COD
(COD) except rate can reach 88.4% -92.54%, 85% -98.14%.
2nd, Regularization activated carbon is good adsorbent first, and Regularization activated carbon and magnetic oxide Fe3O4Micro-
Microwave energy can be absorbed in the presence of ripple and is translated into heat energy, it is higher that the activated centre then formed obtains temperature, most at last
Mineralization of organic material is into CO2And water.
3rd, the mineralization of organic material of charcoal absorption is into CO2After the gas such as water vapour, pore-creating again, recovered part activity,
Improve the utilization rate of activated carbon.
Embodiment
Embodiment 1:
Step A:Clay is obtained after 0.075mm sieves, is soaked in 0.5mol/L -1.0mol/L hydrochloric acid
Half an hour, it is neutral with distilled water filtration and washing to pH, 1h is dried in 60 DEG C of baking oven.
Step B:Clay, Fe3O4, wooden powder absorbent charcoal, copper powder, manganese powder according to mass ratio be 8:21:8:4:7 weigh, and mix
Close uniformly standby.
Step C:Starch quality is with clay quality according to 1:4 are weighed, and a diameter of 0.5mm activity is shaken into after well mixed
Charcoal core, 1h is dried in baking oven at 60 DEG C.
Step D:Obtained activated carbon core in step B and step C and activated charcoal solid powder are mixed, with the pellet rocker system of shaking
Into the initial activity charcoal of Regularization, after drying 1h in 60 DEG C of baking ovens, then take out and be covered in its surface with quartz sand, in Muffle
2h is burnt under conditions of 300 DEG C of stove into Regularization activated carbon.
Regularization activated carbon 2.5g is placed in microwave dissolver with coking chemical waste water made from Example 1 is cleared up, burnt
Change waste water optimum concentration in the range of 180mg/L, the control of the initial pH value of coking chemical waste water is in 8.5, the volume for taking coking chemical waste water
50mL, microwave power is in 600W, exposure time 6min;After resolution reaction cooling terminates, micro-wave diminishing pot is taken out, after processing
Coking chemical waste water filter centrifugation.Coking chemical waste water after filtering is centrifuged under conditions of rotating speed is 500r/min.Coking chemical waste water
After microwave-activated carbon processing, its ammonia nitrogen (NH3- N) and the clearance of COD (COD) respectively reach 85.92%,
80.46%.
Embodiment 2:
Step A:Clay is obtained after 0.075mm sieves, is soaked in 0.5mol/L -1.0mol/L hydrochloric acid
Half an hour, it is neutral with distilled water filtration and washing to pH, 1h is dried in 60 DEG C of baking oven.
Step B:Clay, Fe3O4, wooden powder absorbent charcoal, copper powder, manganese powder according to mass ratio be 8:21:8:4:7 weigh, and mix
Close uniformly standby.
Step C:Starch quality is with clay quality according to 1:4 are weighed, and a diameter of 1mm activated carbon is shaken into after well mixed
Core, 1h is dried in 60 DEG C or so of lower baking oven.
Step D:Obtained activated charcoal solid powder in step B and step C and activated carbon core are mixed, with the pellet rocker system of shaking
Into the initial activity charcoal of Regularization, after drying 1h in 60 DEG C of baking ovens, then take out and be covered in its surface with quartz sand, in Muffle
2h is burnt under conditions of 300 DEG C of stove into Regularization activated carbon.
Regularization activated carbon 2.5g is placed in microwave dissolver with coking chemical waste water made from Example 2 is cleared up, burnt
Change initial pH value control of the waste strength for 180mg/L coking chemical waste waters 8.5, the volume for taking coking chemical waste water is 50mL, microwave work(
Rate is in 650W, exposure time 6min;After resolution reaction cooling terminates, micro-wave diminishing pot is taken out, by the coking chemical waste water after processing
Filter centrifugation.Coking chemical waste water after filtering is centrifuged under conditions of rotating speed is 500r/min.Coking chemical waste water is in microwave-activity
After charcoal processing, its ammonia nitrogen (NH3- N) and the clearance of COD (COD) respectively reach 87.57%, 98.14%.
Claims (9)
- A kind of 1. preparation method for being used to cooperate with the activated carbon of microwave degradation coking chemical waste water, it is characterised in that:Comprise the following steps:Step A:After clay is the higher clay crushing of viscosity, obtained after 0.075mm sieves, i.e. clay particle diameter Small 0.075mm;Wooden powder absorbent charcoal is acidified with hydrochloric acid, after distilled water flushing to neutrality, it is standby to be placed in kept dry in baking oven;Step B:According to mass ratio, clay, Fe made from step A are weighed respectively3O4Powder, wooden powder absorbent charcoal, copper powder and manganese Powder;All solids powder is placed in same container and uniformly mixed;Step C:Take starch to add in clay to be well mixed, a diameter of 0.5mm -1mm spheroid shaken into by the way of water dropwise, Referred to as activated carbon core, the activated carbon core is placed in drying for standby in baking oven;Step D:By obtained activated charcoal solid powder and activated carbon core and mixing in step B and step C, shaken and be made with pellet rocker The initial activity charcoal of Regularization, after drying in baking oven, Muffle furnace burns till Regularization activated carbon.
- 2. a kind of preparation method for being used to cooperate with the activated carbon of microwave degradation coking chemical waste water according to claim 1, it is special Sign is:In described step A, the specific method of wooden powder absorbent charcoal activation is:By wooden powder absorbent charcoal be placed in 0.5mol/L- Half an hour is soaked in 1.0mol/L hydrochloric acid, is neutral with distilled water filtration and washing to pH, is dried in 50 DEG C -80 DEG C of baking oven 1h -2h.
- 3. a kind of preparation method for being used to cooperate with the activated carbon of microwave degradation coking chemical waste water according to claim 1, it is special Sign is:In described step B, clay, Fe3O4Powder, wooden powder absorbent charcoal, copper powder, manganese powder are 8 according to mass ratio:21:8: 4:7 weigh, and are well mixed standby.
- 4. a kind of preparation method for being used to cooperate with the activated carbon of microwave degradation coking chemical waste water according to claim 1, it is special Sign is:In described step C, starch quality is with clay mass ratio according to 1:3–1:4 weigh, and activated carbon core is at 50 DEG C -80 DEG C Baking oven in dry 1h -2h.
- 5. a kind of preparation method for being used to cooperate with the activated carbon of microwave degradation coking chemical waste water according to claim 1, it is special Sign is:In described step D, after the initial activity charcoal of Regularization dries 1h -2h in 50 DEG C of -80 DEG C of baking ovens, then take out Its surface is covered in quartz sand, 2-3h are burnt under conditions of 300 DEG C-400 DEG C of Muffle furnace into Regularization activated carbon.
- A kind of 6. Regularization activated carbon made from claim 1 methods described, it is characterised in that:Obtained Regularization activated carbon contains The mass fraction for having clay is 15% -30%, and wood powder quality of activated carbon fraction is 10% -15%, Fe3O4Mass fraction is 40% -50%, copper powder mass fraction is 15% -20%, and manganese powder mass fraction is 5% -10%.
- 7. the method that Regularization activated carbon made from a kind of claim 1 methods described is handled coking chemical waste water, this method It is:Regularization activated carbon and coking chemical waste water are placed in microwave dissolver and cleared up, after resolution reaction cooling terminates, is taken out Micro-wave diminishing pot, by the coking chemical waste water filter centrifugation after processing.
- 8. processing method according to claim 7, it is characterised in that:The concentration of the coking chemical waste water be 150mg/L- 200mg/L, the initial pH value of coking chemical waste water is 8-10, and the volume ratio of Regularization quality of activated carbon and coking chemical waste water is 1:20–1: 25;Microwave power is 400W -600W, and exposure time is 5min -8min.
- 9. processing method according to claim 7, it is characterised in that:Coking chemical waste water after the filtering is in rotating speed Centrifuged under conditions of 300r/min -500r/min.
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Cited By (2)
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CN109160652A (en) * | 2018-10-29 | 2019-01-08 | 吉林大学 | A kind of method of electrochemistry auxiliary light electrolysis collaboration microwave catalysis processing industrial wastewater |
CN112479518A (en) * | 2020-11-30 | 2021-03-12 | 华东理工大学 | Comprehensive treatment process of cold-rolled aged oil sludge |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109160652A (en) * | 2018-10-29 | 2019-01-08 | 吉林大学 | A kind of method of electrochemistry auxiliary light electrolysis collaboration microwave catalysis processing industrial wastewater |
CN112479518A (en) * | 2020-11-30 | 2021-03-12 | 华东理工大学 | Comprehensive treatment process of cold-rolled aged oil sludge |
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