CN108328598A - A kind of method and carbon material preparing carbon material with petroleum coke using flocculation mud - Google Patents
A kind of method and carbon material preparing carbon material with petroleum coke using flocculation mud Download PDFInfo
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- CN108328598A CN108328598A CN201810016482.8A CN201810016482A CN108328598A CN 108328598 A CN108328598 A CN 108328598A CN 201810016482 A CN201810016482 A CN 201810016482A CN 108328598 A CN108328598 A CN 108328598A
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- carbon material
- petroleum coke
- mud
- flocculation
- flocculation mud
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
Abstract
The invention discloses a kind of methods and carbon material preparing carbon material with petroleum coke using flocculation mud, include the following steps：Step a：The flco drying that dyeing waste water flocculation sediment is obtained, obtains dry flocculation mud；It pulverizes and sieves after dry flocculation mud and petroleum coke are mixed；Then it is vacuum-treated；Step b：The mixture of dry flocculation mud and petroleum coke after vacuum processing is pyrolyzed；Step c：By the pyrogenically prepared black solid ball milling powdering of flco and petroleum coke mixtures；After being added to the stirred tank stirring equipped with deionized water, machine is filtered using sheet frame and is filtered, it is 68 to be washed to filtrate pH value repeatedly；It is finally dried in vacuo, obtains carbon material.Beneficial effects of the present invention:Can by after the Industrial Wastewater Treatment containing dyestuff flco mud and petroleum coke compounding be used as pyrolytic precursors, pyrolysis nitrogen-doped carbon material is prepared, turn waste into wealth, to reach taking into account for both environmental protection and economic extra earning.
Description
Technical field
It is the present invention relates to techniques of Dyeing Wastewater Treatment field, more particularly to a kind of to prepare carbon with petroleum coke using flocculation mud
The method and carbon material of material.
Background technology
Dyeing waste water is the waste water of printing and dyeing mill's discharge based on processing cotton, fiber crops, chemical fibre and its blending product.Printing and dyeing are useless
Water water is larger, and per 100-200 tons of textile water consumption of 1 ton of dyeing and printing process, wherein 80-90% becomes waste water.Textile printing and dyeing wastewater
Have the characteristics that water is big, organic pollution content is high, alkalinity is big, change of water quality is big, belongs to one of intractable industrial wastewater, give up
Contain a large amount of dyestuff and slurry, auxiliary agent, finish, soda acid, fiber impurity, sand substance, inorganic salts etc. in water.
Currently, Industrial Wastewater Treatment mainly has physical treatment, chemical treatment and biological treatment several method.(1) at physics
Reason：The comparison of absorption method in physical method, membrane separation technique method and extraction research is more.(2) it is chemically treated：Chemical flocculation
Method, oxidizing process, electrochemical process etc..Chemical flocculation precipitation method is to be bound to each other to form flocculation using flocculant and Wastewater Pollutant
Body forms precipitation, it is made to remove the pollutant in waste water.Flocculant is divided into inorganic flocculant；Inorganic polymer flocculant；Have
Machine class flocculant；Also some natural macromolecule flocculating agents.Many people are studying new flocculant now, such as present many people
The chitosan flocculant of concern.Electrochemical treatments technology, this method is generally using graphite etc. as cathode, some salt in waste water from dyestuff
Class is as medium, and using some metals etc. as anode, electrochemical degradation is carried out to waste water from dyestuff.But electrochemistry it is of high cost etc. some
Reason examples of industrial application is few.Other emerging technologies, such as advanced oxidation processes, principle is based on the very powerful oxidant of generation
As hydroxyl radical free radical carrys out degradation of contaminant.(3) biological treatment：Microorganism such as bacterium, yeast, algae and fungi etc. can be to dye
Material waste water is degraded.Biodegradation behavior method mainly has fungi decoloration, microbial degradation and biological counter-infiltration system absorption,
Due to technical limitation, biological treatment generally requires a large amount of soil, and is affected by Changes in weather, the limitation of these factors
Its extensive use.
Dyeing waste water flocculates the hazardous waste of mud waste category national regulation, typically contain in these flcos organic matter and
The microorganisms such as toxicity organic element, heavy metal element and pathogen, if being directly entered ecosystem without auxiliary disposition means
System will bring danger, processing that must strictly observe the laws and regulations of country's formulation with disposition to environment and human production activity
Policy.The mode of security landfill generally may be used as final disposal method in flocculation mud, but the method can occupy a large amount of soil
Ground resource, place processing and Seepage are not easy up to standard, the improper secondary pollution that may cause soil of collection control of leachate；
The mud that flocculates can also realize minimizing and innoxious by burning, and burning method is an important hand in addition to landfill
Section.The method is the combined process of pyrolytic and deep oxidation, Flammable Solid Class 4.1 waste oxidation can be made to decompose by burning, reached
To volume, removal toxicity, and recoverable waste heat is reduced, the major defect of burning method is that investment is larger, burning process discharge
Smog causes air secondary pollution, and equipment corrosion phenomenon is serious.Present invention applicant thinks, if flocculation mud can give up
Gurry processing is transformed into high value-added product, not only acts as the purpose to turn waste into wealth, can be this with effective protection environment
Patent application people has carried out correlative study.
Invention content
Technical problem to be solved by the present invention lies in provide a kind of flco by after the Industrial Wastewater Treatment containing dyestuff
As pyrolytic precursors, the method and carbon materials for preparing carbon material with petroleum coke using flocculation mud of the carbon material of high added value are prepared
Material.
In order to solve the above technical problem, the present invention provides a kind of carbon material being prepared with petroleum coke using flocculation mud
Method, wherein the described method comprises the following steps：
Step a：The flco drying that dyeing waste water flocculation sediment is obtained, obtains dry flocculation mud；It flocculates dry
Mud and petroleum coke are according to mass ratio 1:It after 1-6 mixing, is put into high speed disintegrator and crushes, crushed using rotating speed 10000r/min
5-10 minutes, fine powder crossed the sieve of 100-140 mesh；
Then the dry flocculation mud and petroleum coke mixtures that will be obtained, are put into tube furnace, are vacuumized using vacuum pump
To -0.08 to -0.09MPa, argon gas is then passed through to pressure gauge reading as 0 with the flow of 80-150mL/min；Opening is worked off one's feeling vent one's spleen
After valve drives gas in safety flack away, then flowmeter is adjusted to 30-60mL/min；
Step b：The mixture of dry flocculation mud and petroleum coke after vacuum processing is pyrolyzed in tube furnace, heat
Solving program is：It is risen from 20 DEG C using the argon gas for the 30-60mL/min being continually fed into as protection gas with the heating rate of 5 DEG C/min
Temperature is to 800 DEG C, constant temperature 120-300min；Be naturally cooling to room temperature or be cooled to from 800 DEG C with 5 DEG C/min after 400 DEG C again from
It so is cooled to room temperature, obtains black solid powder；
Step c：Dry flocculation mud and the common pyrogenically prepared black solid powder of petroleum coke are milled by ball mill
At the powdery of 120-160 mesh；It is added in the stirred tank equipped with deionized water, the inorganic salts in stirring 8-12h removal carbon materials,
Wherein, the dosage of deionized water is to be diluted using 300-500mL deionized waters per 1g black solids powder；Machine is filtered using sheet frame
It is filtered, it is 6-8 to be washed to filtrate pH value repeatedly；Finally, at a temperature of 50 DEG C -70 DEG C, it is dried in vacuo 8-15h, is obtained
Carbon material.
Wherein, the above method can further include following technical scheme：The step a can also be further：It will
After the flco drying that dyeing waste water flocculation sediment obtains, dry flocculation mud is obtained；Dry flocculation mud and petroleum coke are pressed
According to mass ratio 1:It after 1-6 mixing, is put into high speed disintegrator and crushes, crushed 5-10 minutes using rotating speed 10000r/min, fine powder
Cross the sieve of 100-140 mesh；
Then the dry flocculation mud and petroleum coke mixtures that will be obtained, are put into tube furnace, are vacuumized using vacuum pump
To -0.08 to -0.09MPa, argon gas is then passed through to pressure gauge reading as 0 with the flow of 80-150mL/min；Then it recycles
Vacuum pump is evacuated to -0.08 to -0.09MPa, then is passed through argon gas to pressure gauge reading with the flow of 80-150mL/min as 0,
In triplicate；4th time by argon gas be passed through to pressure gauge reading be 0 when, open outlet air valve gas in safety flack is driven away after,
Flowmeter is adjusted again to 30-60mL/min.
Wherein, the above method can further include following technical scheme：In the step a, flco is at 80-150 DEG C
Forced air drying 40-50h is ground into 100-140 mesh powders, then with 60-90 DEG C of vacuum drying 5-15h, obtains dry flocculation and become silted up
Mud.
Wherein, the above method can further include following technical scheme：The pyrolysis procedure of the step b can also be into
One step is：It is heated up from 20 DEG C using the argon gas for the 30-60mL/min being continually fed into as protection gas with the heating rate of 5 DEG C/min
To 300-400 DEG C, constant temperature 60-90min；Again with the heating rate of 5 DEG C/min, 800 DEG C are warming up to from 300-400 DEG C, it is then permanent
Warm 120-240min；Finally be naturally cooling to room temperature or with 5 DEG C/min from 800 DEG C be cooled to 400 DEG C after be naturally cooling to again
Room temperature obtains black solid powder.
Wherein, the above method can further include following technical scheme：Before the step a can also include with
Lower step, step d：The pH value of dyeing waste water is adjusted to 4-10, flocculant is then added into dyeing waste water, stands one day,
Supernatant liquid is removed, centrifugal treating is carried out to lower layer's solid, the rotating speed of centrifugation is 3000-5000rpm, centrifugation time 5-
15min obtains flco.
Wherein, the above method can further include following technical scheme：In the step d, the flocculant and institute
The mass ratio for stating the dyestuff in dyeing waste water is 1:The additive amount of 2-2.5 or described flocculants is 7-25g/L.
In addition, the present invention still further provides and a kind of utilizes above-mentioned any one using flocculation mud and petroleum coke system
The carbon material that the method for standby carbon material is prepared.I.e. a kind of carbon material prepared with petroleum coke using flocculation mud, wherein its
Preparation method includes the following steps：
Step a：The flco drying that dyeing waste water flocculation sediment is obtained obtains dry flocculation mud；Flco is dried and is wadded a quilt with cotton
Solidifying mud and petroleum coke are according to mass ratio 1:After 1-6 mixing, it is put into high speed disintegrator and crushes, using rotating speed 10000r/min powder
5-10 minutes broken, fine powder crosses the sieve of 100-140 mesh；
Then dry flocculation mud and petroleum coke are put into tube furnace, using vacuum pump be evacuated to -0.08 to -
Then 0.09MPa is passed through argon gas to pressure gauge reading as 0 with the flow of 80-150mL/min；Outlet air valve is opened by safety flack
After interior gas is driven away, then flowmeter is adjusted to 30-60mL/min；
Step b：Heat is carried out in tube furnace to the mixture of flco drying flocculation mud and petroleum coke after vacuum processing
Solution, pyrolysis procedure are：With the heating rate of 5 DEG C/min, using the argon gas for the 30-60mL/min being continually fed into as protection gas, from
20 DEG C are warming up to 800 DEG C, constant temperature 120-300min；It is naturally cooling to room temperature or is cooled to 400 DEG C from 800 DEG C with 5 DEG C/min
It is naturally cooling to room temperature again afterwards, obtains black solid powder；
Step c：Flco is dried into flocculation mud and the common pyrogenically prepared black solid powder of petroleum coke passes through ball mill
It is milled into the powdery of 120-160 mesh；It is added in the stirred tank equipped with deionized water, the nothing in stirring 8-12h removal carbon materials
Machine salt, wherein the dosage of deionized water is to be diluted using 300-500mL deionized waters per 1g black solids powder；Using sheet frame
Suction filtration machine is filtered, and it is 6-8 to be washed to filtrate pH value repeatedly；Finally, at a temperature of 50 DEG C -70 DEG C, it is dried in vacuo 8-
15h obtains carbon material.
Wherein, the above method can further include following technical scheme：The step a can also be further：It will
After the flco drying that dyeing waste water flocculation sediment obtains, dry flocculation mud is obtained；Flco is dried into flocculation mud and petroleum coke
According to mass ratio 1:It after 1-6 mixing, is put into high speed disintegrator and crushes, using rotating speed 10000r/min crushing 5-10 minutes, carefully
Powder crosses the sieve of 100-140 mesh；
Then dry flocculation mud and petroleum coke are put into tube furnace, using vacuum pump be evacuated to -0.08 to -
Then 0.09MPa is passed through argon gas to pressure gauge reading as 0 with the flow of 80-150mL/min；Then recycle vacuum pumping true
It is empty to be passed through argon gas to pressure gauge reading for 0, in triplicate to -0.08 to -0.09MPa, then with the flow of 80-150mL/min；The
Four times by argon gas be passed through to pressure gauge reading be 0 when, open after outlet air valve drives gas in safety flack away, then adjust flowmeter
To 30-60mL/min.
Wherein, the above method can further include following technical scheme：In the step a, flco is at 80-150 DEG C
Forced air drying 40-50h is ground into 100-140 mesh powders, then with 60-90 DEG C of vacuum drying 5-15h, obtains dry flocculation and become silted up
Mud.
Wherein, the above method can further include following technical scheme：The pyrolysis procedure of the step b can also be into
One step is：It is heated up from 20 DEG C using the argon gas for the 30-60mL/min being continually fed into as protection gas with the heating rate of 5 DEG C/min
To 300-400 DEG C, constant temperature 60-90min；Again with the heating rate of 5 DEG C/min, 800 DEG C are warming up to from 300-400 DEG C, it is then permanent
Warm 120-240min；Finally be naturally cooling to room temperature or with 5 DEG C/min from 800 DEG C be cooled to 400 DEG C after be naturally cooling to again
Room temperature obtains black solid powder.
Wherein, the above method can further include following technical scheme：Before the step a can also include with
Lower step, step d：The pH value of dyeing waste water is adjusted to 4-10, flocculant is then added into dyeing waste water, stands one day,
Supernatant liquid is removed, centrifugal treating is carried out to lower layer's solid, the rotating speed of centrifugation is 3000-5000rpm, centrifugation time 5-
15min obtains flco.
Wherein, the above method can further include following technical scheme：In the step d, the flocculant and institute
The mass ratio for stating the dyestuff in dyeing waste water is 1:The additive amount of 2-2.5 or described flocculants is 7-25g/L.
In addition, the present invention has been still further provided in a kind of ultracapacitor being prepared using above-mentioned carbon material；System
The method of standby ultracapacitor is the art common method, and the carbon material only used is to be flocculated mud with above-mentioned utilization
The carbon material that the method for preparing carbon material with petroleum coke is prepared.
In addition, the present invention has been still further provided in a kind of oxygen reduction catalyst being prepared using above-mentioned carbon material；
The method for preparing oxygen reduction catalyst is the art common method, and the carbon material only used is with above-mentioned utilization flocculation
The carbon material that mud is prepared with the method that petroleum coke prepares carbon material.
In addition, the present invention has been still further provided in a kind of activated carbon being prepared using above-mentioned carbon material；It prepares and lives
Property charcoal method be the art common method, the carbon material only used is to be flocculated mud and petroleum coke with above-mentioned utilization
The carbon material that the method for preparing carbon material is prepared.
Beneficial effects of the present invention:The method that the present invention prepares carbon material using flocculation mud with petroleum coke, can will contain
It is used as pyrolytic precursors, pyrolysis that N doping is prepared after having the flco mud after the Industrial Wastewater Treatment of dyestuff and petroleum coke compounding
Carbon material, while the pollutant for including the noxious materials such as dyestuff, heavy metal, aromatic hydrocarbons in industrial wastewater has been handled well, it will give up
It abandons flocculation mud and petroleum coke is changed into the carbon material of high added value, the carbon material being prepared can be good at applying super
The fields such as capacitor and elctro-catalyst, to reach taking into account for both environmental protection and economic extra earning.The present invention's utilizes flocculation
The method that mud prepares carbon material with petroleum coke, may be used positive ion organic high polymer coagulant to printing and dyeing mill's high-colour intensity wastewater
It carries out taking off steady settlement treatment, it can also be used to weave, the place of the high chromaticity industrial waste waters such as pigment, ink, black liquid, oil drilling
Then discarded flocculation mud and petroleum coke mixtures are obtained three-dimensional porous carbon material by reason through pyrolysis.The principle of the method for the present invention
It is that organic polymer coargulator can be used as carbon source, organic dyestuff that can provide abundant nitrogen source, petroleum coke can provide rich
Rich carbon source realizes that nitrogen source is successfully entrained in carbon material by high temperature pyrolysis and obtains nitrogen-doped carbon material.
Description of the drawings
Fig. 1 is the SEM (a, b) and TEM (c, d) image of the carbon material of the embodiment of the present invention 1 and 2；
Fig. 2 is the Pore Characterization figure of the porous carbon materials of the embodiment of the present invention 1 and 2；
Fig. 3 is that the XPS of the carbon material of the embodiment of the present invention 1 and 2 composes (a), high-resolution N1s (b), C1s (c) and O1s (d) entirely
The collection of illustrative plates that deconvolutes；
Fig. 4 is the SEM-mapping images of C, N and the O element of the carbon material of the embodiment of the present invention 1 and 2；
Fig. 5 is electrode material performance map of the carbon material of the embodiment of the present invention 1 and 2 under three-electrode system.
Fig. 6 is electrode material performance map of the carbon material of the embodiment of the present invention 3 and 4 under three-electrode system.
Fig. 7 is electrode material performance map of the carbon material of the embodiment of the present invention 5 and 6 under three-electrode system.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment to the present invention
Embodiment is described in further detail.
Embodiment 1：The embodiment of the invention discloses a kind of method preparing carbon material with petroleum coke using flocculation mud, packets
Include following steps：
Step d：Waste water from dyestuff comes from local printing and dyeing enterprise, takes 5L waste water from dyestuff, and dye strength is 200ppm when flocculation, is adjusted
Save pH value of solution=8.5；Be added into waste water from dyestuff cationic flocculant BADT-CTS (2,4- bis- (diformazan ammonia) -6- it is chloro- [1,3,
5]-triazine radical chitosan ether, flocculant concentration control stand one day in 9g/L, remove supernatant liquid, to lower layer's solid carry out from
Heart processing accelerates to be separated by solid-liquid separation, and centrifugal rotational speed 4500rpm, centrifugation time 15min obtain solid flco.
Step a：120 mesh powder are ground into, at 60 DEG C with 100 DEG C of forced air drying 45h to the solid flco that step d is obtained
It is dried in vacuo 6h, obtains dry flocculation mud；It takes flco drying flocculation mud 100g to be mixed with 100g petroleum cokes, is put into high speed powder
It crushes, is crushed 5 minutes using rotating speed 10000r/min, fine powder crosses the sieve of 120 mesh in broken machine.
The dry flocculation mud and petroleum coke mixtures that will be obtained, are put into tube furnace, be evacuated to using vacuum pump-
Then 0.09MPa is passed through argon gas to pressure gauge reading as 0 with the flow of 100mL/min；Outlet air valve is opened by gas in safety flack
After body is driven away, then flowmeter is adjusted to 40mL/min；
Step b：The mixture of dry flocculation mud and petroleum coke is pyrolyzed in tube furnace, pyrolysis procedure is：With
The argon gas for the 40mL/min being continually fed into is warming up to 300 DEG C from 20 DEG C as protection gas, with the heating rate of 5 DEG C/min, keeps
72min is warming up to 800 DEG C with the heating rate of 5 DEG C/min later, keeps 138min.Final sample is naturally cooling to room temperature, obtains
To black solid powder.
Step c：Black solid powder made from flco and petroleum coke altogether heat is milled into 140 mesh powderies by ball mill；
It is added in the stirred tank equipped with deionized water, the inorganic salts in stirring 10h removal carbon materials, wherein the dosage of deionized water
It is diluted using 400mL deionized waters for every 1g black solids powder；Machine is filtered using sheet frame to be filtered, and is washed to filtrate repeatedly
PH value is 7；Finally, at a temperature of 60 DEG C, it is dried in vacuo 10h, obtains carbon material.
Embodiment 2：The embodiment of the invention discloses a kind of carbon materials prepared with petroleum coke using flocculation mud, prepare
Method includes the following steps：
Step d：Waste water from dyestuff comes from local printing and dyeing enterprise, takes 5L waste water from dyestuff, and dye strength is 200ppm when flocculation, is adjusted
Save pH value of solution=8.5；Be added into waste water from dyestuff cationic flocculant BADT-CTS (2,4- bis- (diformazan ammonia) -6- it is chloro- [1,3,
5]-triazine radical chitosan ether, flocculant concentration control stand one day in 9g/L, remove supernatant liquid, to lower layer's solid carry out from
Heart processing accelerates to be separated by solid-liquid separation, and centrifugal rotational speed 4500rpm, centrifugation time 15min obtain solid flco.
Step a：120 mesh powder are ground into, at 60 DEG C with 100 DEG C of forced air drying 45h to the solid flco that step d is obtained
It is dried in vacuo 6h, obtains dry flocculation mud；It takes flco drying flocculation mud 100g to be mixed with 100g petroleum cokes, is put into high speed powder
It crushes, is crushed 5 minutes using rotating speed 10000r/min, fine powder crosses the sieve of 120 mesh in broken machine.
Obtained dry flocculation mud and petroleum coke are put into tube furnace, -0.09MPa is evacuated to using vacuum pump,
Then argon gas is passed through to pressure gauge reading as 0 with the flow of 100mL/min；Outlet air valve is opened to drive gas in safety flack away
Afterwards, then flowmeter is adjusted to 30-60mL/min；
Step b：Heat is carried out in tube furnace to the mixture of flco drying flocculation mud and petroleum coke after vacuum processing
Solution, pyrolysis procedure are：Using the argon gas for the 30-60mL/min being continually fed into as protection gas, with the heating rate of 5 DEG C/min from 20
300 DEG C DEG C are warming up to, 72min is kept, is warming up to 800 DEG C later with the heating rate of 5 DEG C/min, keeps 138min.Last sample
Product are naturally cooling to room temperature, obtain black solid powder.
Step c：Flco is dried black solid powder made from flocculation mud and the total heat of petroleum coke to mill by ball mill
At 140 mesh powderies；It is added in the stirred tank equipped with deionized water, the inorganic salts in stirring 10h removal carbon materials, wherein go
The dosage of ionized water is to be diluted using 400mL deionized waters per 1g black solids powder；Machine is filtered using sheet frame to be filtered, instead
It is 7 that rehydration, which is washed till filtrate pH value,；Finally, at a temperature of 60 DEG C, it is dried in vacuo 10h, obtains carbon material.
The carbon material being prepared using the method for Examples 1 and 2, after tested, performance are shown in Fig. 1-Fig. 4.
Fig. 1 is the porous shape appearance figure of the carbon material of the embodiment of the present invention 1 and 2, wherein (a) and (b) are SEM image, (c) and
(d) it is TEM image.From fig. 1, it can be seen that the porous carbon sample prepared forms the hole path of connection.
Fig. 2 is the Pore Characterization of the porous carbon materials of the embodiment of the present invention 1 and 2, wherein Fig. 2 (a) is porous carbon materials
Nitrogen De contamination curve, Fig. 2 (b) be Kong Rong-pore-size distribution image, the Raman images that Fig. 2 (c) is porous carbon materials and Fig. 2
(d) it is XRD spectrum.Shown in Fig. 2, porous carbon sample shows the adsorption isotherm of IV type, and relevant pore structure parameter is, than
Surface area：1254m2/g, pore volume：0.603cm3/ g, average pore size：5.9nm.In addition, there is apparent carbon material in sample
Diffraction maximum, and containing a small amount of graphitized carbon structure.It can be seen that sample has porous structure simultaneously from XRD and Raman
And distribution of pores it is wider, but sample degree of graphitization is relatively low, and defect is more.
Fig. 3 is that the XPS of porous carbon materials of the embodiment of the present invention 1 and 2 compose (a) entirely, high-resolution N1s (b), C1s (c) with
The collection of illustrative plates that deconvolutes of O1s (d), as can be seen from Figure 3, C, O in the porous carbon materials of the embodiment of the present invention 1 and N element content difference
For：81.9%, 8.7% and 9.4%, thus there is N, the characteristics of O codopes.
Fig. 4 is the SEM-mapping images of the porous carbon materials of the embodiment of the present invention 1 and 2, is further demonstrated in sample
Each element is evenly distributed.
Using the super electrical property for the carbon material that the method for Examples 1 and 2 is prepared, after tested, performance is shown in Fig. 5.
Fig. 5 is the performance map of electrode material of the porous carbon materials of the embodiment of the present invention 1 and 2 under three-electrode system, tool
Body is CV image of the porous carbon materials in 6MKOH solution.Wherein, the super electric performance test sample preparation methods of carbon material are：
Foam nickel screen is cut into (20mm*10mm) strip, then the ultrasound 10min processing in acetone and dilute hydrochloric acid respectively, last 80 DEG C
Vacuum drying.Then the carbon material that embodiment 1 or 2 is prepared is pressed with carbon black and 6wt% Kynoar solutions (PVDF)
According to mass ratio 8:1:1 ratio is dispersed in N-Methyl pyrrolidone (NMP), is stirred overnight.Then the black paste that will be obtained
Coating substance on processed nickel screen, 120 DEG C vacuum drying 8h.Then, apply on dried sample
The power of 10MPa.The active material of each working electrode is about 3mg.Wherein, super electric property assessment：In 6.0MKOH, three are carried out
The electro-chemical test of electrode system.In entire test process, Hg/Hg2Cl2As reference electrode, Pt paillons (1cm2) conduct pair
Electrode.Peace volt-ampere curve (CV) is followed to carry out on electrochemical workstation.
From fig. 5, it can be seen that test its capacitance can reach 138F/g in 5mV/s.Therefore, the flocculation that we use is become silted up
Mud compounds the carbon material obtained as precursor with petroleum coke and is obtained with commercial other presomas (coconut husk, petroleum coke, chitosan etc.)
The super electrical property arrived is close.
Embodiment 3：The embodiment of the invention discloses a kind of method preparing carbon material with petroleum coke using flocculation mud, packets
Include following steps：
Step d：Waste water from dyestuff comes from local printing and dyeing enterprise, takes 5L waste water from dyestuff, and dye strength is 500ppm when flocculation, is adjusted
Save pH value of solution=7.5；Be added into waste water from dyestuff cationic flocculant BADT-CTS (2,4- bis- (diformazan ammonia) -6- it is chloro- [1,3,
5]-triazine radical chitosan ether, flocculant concentration control stand one day in 12g/L, remove supernatant liquid, carried out to lower layer's solid
Centrifugal treating accelerates to be separated by solid-liquid separation, and centrifugal rotational speed 4200rpm, centrifugation time 12min obtain solid flco.
Step a：110 mesh powder are ground into, at 75 DEG C with 105 DEG C of forced air drying 42h to the solid flco that step d is obtained
It is dried in vacuo 8h, obtains dry flocculation mud；It takes flco drying flocculation mud 100g to be mixed with 200g petroleum cokes, is put into high speed powder
It crushes, is crushed 6 minutes using rotating speed 10000r/min, fine powder crosses the sieve of 130 mesh in broken machine.
The dry flocculation mud and petroleum coke mixtures that will be obtained, are put into tube furnace, be evacuated to using vacuum pump-
Then 0.09MPa is passed through argon gas to pressure gauge reading as 0 with the flow of 140mL/min；Then vacuum pump is recycled to vacuumize
Argon gas is passed through to pressure gauge reading for 0, in triplicate to -0.09MPa, then with the flow of 140mL/min；4th time argon gas is led to
Enter to pressure gauge reading be 0 when, open after outlet air valve drives gas in safety flack away, then adjust flowmeter to 55mL/min；
Step b：The mixture of dry flocculation mud and petroleum coke after vacuum processing is pyrolyzed in tube furnace, heat
Solving program is：Using the argon gas for the 55mL/min being continually fed into as protection gas, it is warming up to from 20 DEG C with the heating rate of 5 DEG C/min
800 DEG C, keep 200min.Finally with 5 DEG C/min from 800 DEG C be cooled to 400 DEG C after be naturally cooling to room temperature again, it is solid to obtain black
Body powder.
Step c：Black solid powder made from flco and petroleum coke altogether heat is milled into 140 mesh powderies by ball mill；
It is added in the stirred tank equipped with deionized water, the inorganic salts in stirring 11h removal carbon materials, wherein the dosage of deionized water
It is diluted using 360mL deionized waters for every 1g black solids powder；Machine is filtered using sheet frame to be filtered, and is washed to filtrate repeatedly
PH value is 7.5；Finally, at a temperature of 65 DEG C, it is dried in vacuo 12h, obtains carbon material.
Embodiment 4：The embodiment of the invention discloses a kind of carbon materials prepared with petroleum coke using flocculation mud, prepare
Method includes the following steps：
Step d：Waste water from dyestuff comes from local printing and dyeing enterprise, takes 5L waste water from dyestuff, and dye strength is 500ppm when flocculation, is adjusted
Save pH value of solution=7.5；Be added into waste water from dyestuff cationic flocculant BADT-CTS (2,4- bis- (diformazan ammonia) -6- it is chloro- [1,3,
5]-triazine radical chitosan ether, flocculant concentration control stand one day in 12g/L, remove supernatant liquid, carried out to lower layer's solid
Centrifugal treating accelerates to be separated by solid-liquid separation, and centrifugal rotational speed 4200rpm, centrifugation time 12min obtain solid flco.
Step a：110 mesh powder are ground into, at 75 DEG C with 105 DEG C of forced air drying 42h to the solid flco that step d is obtained
It is dried in vacuo 8h, obtains dry flocculation mud；It takes flco drying flocculation mud 100g to be mixed with 200g petroleum cokes, is put into high speed powder
It crushes, is crushed 6 minutes using rotating speed 10000r/min, fine powder crosses the sieve of 130 mesh in broken machine.
The dry flocculation mud and petroleum coke mixtures that will be obtained, are put into tube furnace, be evacuated to using vacuum pump-
Then 0.09MPa is passed through argon gas to pressure gauge reading as 0 with the flow of 140mL/min；Then vacuum pump is recycled to vacuumize
Argon gas is passed through to pressure gauge reading for 0, in triplicate to -0.09MPa, then with the flow of 140mL/min；4th time argon gas is led to
Enter to pressure gauge reading be 0 when, open after outlet air valve drives gas in safety flack away, then adjust flowmeter to 55mL/min；
Step b：The mixture of dry flocculation mud and petroleum coke after vacuum processing is pyrolyzed in tube furnace, heat
Solving program is：Using the argon gas for the 55mL/min being continually fed into as protection gas, it is warming up to from 20 DEG C with the heating rate of 5 DEG C/min
800 DEG C, keep 200min.Finally with 5 DEG C/min from 800 DEG C be cooled to 400 DEG C after be naturally cooling to room temperature again, it is solid to obtain black
Body powder.
Step c：Black solid powder made from flco and petroleum coke altogether heat is milled into 140 mesh powderies by ball mill；
It is added in the stirred tank equipped with deionized water, the inorganic salts in stirring 11h removal carbon materials, wherein the dosage of deionized water
It is diluted using 360mL deionized waters for every 1g black solids powder；Machine is filtered using sheet frame to be filtered, and is washed to filtrate repeatedly
PH value is 7.5；Finally, at a temperature of 65 DEG C, it is dried in vacuo 12h, obtains carbon material.
Using the super electrical property for the carbon material that the method for embodiment 3 and 4 is prepared, after tested, performance is shown in Fig. 6.
Fig. 6 is the performance map of electrode material of the porous carbon materials of the embodiment of the present invention 3 and 4 under three-electrode system.Its
In, Fig. 6 (a) is CV image of the porous carbon materials in 6MKOH solution；Fig. 6 (b) is the constant current charge-discharge diagram of porous carbon materials
Picture.Wherein, the super electric performance test sample preparation methods of carbon material are：Foam nickel screen is cut into (20mm*10mm) strip, then
The ultrasound 10min processing in acetone and dilute hydrochloric acid respectively, last 80 DEG C of vacuum drying.Then embodiment 3 or 4 is prepared
Carbon material is with carbon black and 6wt% Kynoar solutions (PVDF) according to mass ratio 8:1:1 ratio is dispersed in N- methylpyrroles
In alkanone (NMP), it is stirred overnight.Then by the coating substance of obtained black paste on processed nickel screen, 120 DEG C
It is dried in vacuo 8h.Then, apply the power of 10MPa on dried sample.Each the active material of working electrode is about
3mg.Wherein, super electric property assessment：In 6.0MKOH, the electro-chemical test of three-electrode system is carried out.In entire test process
In, Hg/Hg2Cl2As reference electrode, Pt paillons (1cm2) as to electrode.Constant current charge-discharge curve (GCD) and follow peace volt-ampere
Curve (CV) and cyclical stability carry out on electrochemical workstation.
From Fig. 6 (b) it can be seen that test its capacitance can reach 255F/g in 5mV/s.Therefore, the flocculation that we use
Mud compounds the carbon material obtained as precursor and commercial other presomas (coconut husk, petroleum coke, chitosan etc.) with petroleum coke
Obtained super electrical property is close.
Embodiment 5：The embodiment of the invention discloses a kind of method preparing carbon material with petroleum coke using flocculation mud, packets
Include following steps：
Step d：Waste water from dyestuff comes from local printing and dyeing enterprise, takes 5L waste water from dyestuff, and dye strength is 2000ppm when flocculation,
Adjust pH value of solution=8.5；Be added into waste water from dyestuff cationic flocculant BADT-CTS (2,4- bis- (diformazan ammonia) -6- it is chloro- [1,
3,5]-triazine radical chitosan ether, flocculant concentration 20g/L, stand one day, remove supernatant liquid, to lower layer's solid carry out from
Heart processing accelerates to be separated by solid-liquid separation, and centrifugal rotational speed 5000rpm, centrifugation time 13min obtain solid flco.
Step a：100 mesh powder are ground into, at 85 DEG C with 110 DEG C of forced air drying 48h to the solid flco that step d is obtained
It is dried in vacuo 9h, obtains dry flocculation mud；It takes flco drying flocculation mud 100g to be mixed with 500g petroleum cokes, is put into high speed powder
It crushes, is crushed 8 minutes using rotating speed 10000r/min, fine powder crosses the sieve of 120 mesh in broken machine.
The dry flocculation mud and petroleum coke mixtures that will be obtained, are put into tube furnace, be evacuated to using vacuum pump-
Then 0.08MPa is passed through argon gas to pressure gauge reading as 0 with the flow of 80mL/min；Outlet air valve is opened by gas in safety flack
After body is driven away, then flowmeter is adjusted to 35mL/min；
Step b：The mixture of dry flocculation mud and petroleum coke after vacuum processing is pyrolyzed in tube furnace, heat
Solving program is：Using the argon gas for the 35mL/min being continually fed into as protection gas, it is warming up to from 20 DEG C with the heating rate of 5 DEG C/min
350 DEG C, 85min is kept, then 800 DEG C are warming up to the heating rate of 5 DEG C/min, keep 160min.Final sample Temperature fall
To room temperature, black solid powder is obtained.
Step c：Black solid powder made from flco and petroleum coke altogether heat is milled into 150 mesh powderies by ball mill；
It is added in the stirred tank equipped with deionized water, the inorganic salts in stirring 9.5h removal carbon materials, wherein the dosage of deionized water
It is diluted using 420mL deionized waters for every 1g black solids powder；Machine is filtered using sheet frame to be filtered, and is washed to filtrate repeatedly
PH value is 6.8；Finally, at a temperature of 70 DEG C, it is dried in vacuo 9.5h, obtains carbon material.
Embodiment 6：The embodiment of the invention discloses a kind of carbon materials prepared with petroleum coke using flocculation mud, prepare
Method includes the following steps：
Step d：Waste water from dyestuff comes from local printing and dyeing enterprise, takes 5L waste water from dyestuff, and dye strength is 2000ppm when flocculation,
Adjust pH value of solution=8.5；Be added into waste water from dyestuff cationic flocculant BADT-CTS (2,4- bis- (diformazan ammonia) -6- it is chloro- [1,
3,5]-triazine radical chitosan ether, flocculant concentration 20g/L, stand one day, remove supernatant liquid, to lower layer's solid carry out from
Heart processing accelerates to be separated by solid-liquid separation, and centrifugal rotational speed 5000rpm, centrifugation time 13min obtain solid flco.
Step a：100 mesh powder are ground into, at 85 DEG C with 110 DEG C of forced air drying 48h to the solid flco that step d is obtained
It is dried in vacuo 9h, obtains dry flocculation mud；It takes flco drying flocculation mud 100g to be mixed with 500g petroleum cokes, is put into high speed powder
It crushes, is crushed 8 minutes using rotating speed 10000r/min, fine powder crosses the sieve of 120 mesh in broken machine.
The dry flocculation mud and petroleum coke mixtures that will be obtained, are put into tube furnace, be evacuated to using vacuum pump-
Then 0.08MPa is passed through argon gas to pressure gauge reading as 0 with the flow of 80mL/min；Outlet air valve is opened by gas in safety flack
After body is driven away, then flowmeter is adjusted to 35mL/min；
Step b：The mixture of dry flocculation mud and petroleum coke after vacuum processing is pyrolyzed in tube furnace, heat
Solving program is：Using the argon gas for the 35mL/min being continually fed into as protection gas, it is warming up to from 20 DEG C with the heating rate of 5 DEG C/min
350 DEG C, 85min is kept, then 800 DEG C are warming up to the heating rate of 5 DEG C/min, keep 160min.Final sample Temperature fall
To room temperature, black solid powder is obtained.
Step c：Black solid powder made from flco and petroleum coke altogether heat is milled into 150 mesh powderies by ball mill；
It is added in the stirred tank equipped with deionized water, the inorganic salts in stirring 9.5h removal carbon materials, wherein the dosage of deionized water
It is diluted using 420mL deionized waters for every 1g black solids powder；Machine is filtered using sheet frame to be filtered, and is washed to filtrate repeatedly
PH value is 6.8；Finally, at a temperature of 70 DEG C, it is dried in vacuo 9.5h, obtains carbon material.
Using the super electrical property for the carbon material that the method for embodiment 5 and 6 is prepared, after tested, performance is shown in Fig. 7.
Fig. 7 is the performance map of electrode material of the porous carbon materials of the embodiment of the present invention 5 and 6 under three-electrode system.Its
In, (a) is CV image of the porous carbon materials in 6MKOH solution；(b) it is the constant current charge-discharge image of porous carbon materials.Wherein,
The super electric performance test sample preparation methods of carbon material are：Foam nickel screen is cut into (20mm*10mm) strip, then respectively third
Ultrasound 10min processing in ketone and dilute hydrochloric acid, last 80 DEG C of vacuum drying.Then the carbon material that embodiment 5 or 6 is prepared with
Carbon black and 6wt% Kynoar solutions (PVDF) are according to mass ratio 8:1:1 ratio is dispersed in N-Methyl pyrrolidone (NMP)
In, it is stirred overnight.Then by the coating substance of obtained black paste on processed nickel screen, 120 DEG C of vacuum drying
8h.Then, apply the power of 10MPa on dried sample.The active material of each working electrode is about 3mg.Wherein,
Super electric property assessment：In 6.0MKOH, the electro-chemical test of three-electrode system is carried out.In entire test process, Hg/Hg2Cl2
As reference electrode, Pt paillons (1cm2) as to electrode.Constant current charge-discharge curve (GCD) and follow peace volt-ampere curve (CV), with
And cyclical stability carries out on electrochemical workstation.
Shown in Fig. 7 (b), tests its capacitance and can reach 266F/g in 5mV/s.Therefore, what we used contains dyestuff
The obtained carbon material of flco it is close with the super electrical property that commercial other presomas (coconut husk, petroleum coke, chitosan etc.) obtain.
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But it is every without departing from technical solution of the present invention content, according to the technical essence of the invention to above example institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection domain of technical solution of the present invention.
Claims (10)
1. a kind of method preparing carbon material with petroleum coke using flocculation mud, which is characterized in that the method includes following steps
Suddenly：
Step a：After the flco drying that dyeing waste water flocculation sediment is obtained, dry flocculation mud is obtained；By the dry mud that flocculates
With petroleum coke according to mass ratio 1:It after 1-6 mixing, is put into high speed disintegrator and crushes, 5-10 is crushed using rotating speed 10000r/min
Minute, fine powder crosses the sieve of 100-140 mesh；
The dry flocculation mud and petroleum coke mixtures that will be obtained, are put into tube furnace, -0.08 are evacuated to using vacuum pump
To -0.09MPa, argon gas is then passed through to pressure gauge reading as 0 with the flow of 80-150mL/min；Opening outlet air valve will be safe
After gas is driven away in bottle, then flowmeter is adjusted to 30-60mL/min；
Step b：The mixture of dry flocculation mud and petroleum coke after vacuum processing is pyrolyzed in tube furnace, is pyrolyzed journey
Sequence is：It is warming up to from 20 DEG C using the argon gas for the 30-60mL/min being continually fed into as protection gas with the heating rate of 5 DEG C/min
800 DEG C, constant temperature 120-300min；It is naturally cooling to room temperature or is cooled to after 400 DEG C from 800 DEG C with 5 DEG C/min drop naturally again
It warms to room temperature, obtains black solid powder；
Step c：Dry flocculation mud and the common pyrogenically prepared black solid powder of petroleum coke are milled by ball mill
The powdery of 120-160 mesh；It is added in the stirred tank equipped with deionized water, the inorganic salts in stirring 8-12h removal carbon materials,
In, the dosage of deionized water is to be diluted using 300-500mL deionized waters per 1g black solids powder；Using sheet frame filter machine into
Row filters, and it is 6-8 to be washed to filtrate to pH value repeatedly；Finally, at a temperature of 50 DEG C -70 DEG C, it is dried in vacuo 8-15h, is obtained
Carbon material.
2. the method as described in claim 1 for preparing carbon material with petroleum coke using flocculation mud, which is characterized in that the step
Suddenly a can also be further：After the flco drying that dyeing waste water flocculation sediment is obtained, dry flocculation mud is obtained；It will do
Dry flocculation mud and petroleum coke are according to mass ratio 1:After 1-6 mixing, it is put into high speed disintegrator and crushes, using rotating speed 10000r/
Min is crushed 5-10 minutes, and fine powder crosses the sieve of 100-140 mesh；
The dry flocculation mud and petroleum coke mixtures that will be obtained, are put into tube furnace, -0.08 are evacuated to using vacuum pump
To -0.09MPa, argon gas is then passed through to pressure gauge reading as 0 with the flow of 80-150mL/min；Then vacuum pumping is recycled
Vacuum is passed through argon gas to pressure gauge reading for 0, in triplicate to -0.08 to -0.09MPa, then with the flow of 80-150mL/min；
4th time by argon gas be passed through to pressure gauge reading be 0 when, open after outlet air valve drives gas in safety flack away, then adjust flow
It counts to 30-60mL/min.
3. the method as claimed in claim 1 or 2 for preparing carbon material with petroleum coke using flocculation mud, which is characterized in that institute
It states in step a, to forced air drying 40-50h at a temperature of 80-150 DEG C of flco, is ground into 100-140 mesh powders, then 60-90 DEG C
At a temperature of be dried in vacuo 5-15h, obtain dry flocculation mud.
4. the method for preparing carbon material with petroleum coke using flocculation mud as described in claims 1 to 3 is any, feature exist
In the pyrolysis procedure of the step b can also be further：With the heating rate of 5 DEG C/min, with the 30-60mL/ being continually fed into
The argon gas of min is warming up to 300-400 DEG C from 20 DEG C, constant temperature 60-90min as protection gas；Again with the heating rate of 5 DEG C/min,
800 DEG C are warming up to from 300-400 DEG C, then constant temperature 120-240min；Finally be naturally cooling to room temperature or with 5 DEG C/min from
800 DEG C be cooled to 400 DEG C after be naturally cooling to room temperature again, obtain black solid powder.
5. the method for preparing carbon material with petroleum coke using flocculation mud as described in Claims 1-4 is any, feature exist
In can also include the following steps before the step a, step d：The pH value of dyeing waste water is adjusted to 4-10, then to
Flocculant is added in dyeing waste water, stands one day, removes supernatant liquid, centrifugal treating, the rotating speed of centrifugation are carried out to lower layer's solid
Flco is obtained for 3000-5000rpm, centrifugation time 5-15min.
6. the method as claimed in claim 5 for preparing carbon material with petroleum coke using flocculation mud, which is characterized in that the step
In rapid d, the mass ratio of the flocculant and the dyestuff in the dyeing waste water is 1:The additive amount of 2-2.5 or described flocculants
For 7-25g/L.
7. a kind of carbon material being prepared using any the method for claim 1 to 6.
8. a kind of ultracapacitor that the carbon material being prepared using any the method for claim 1 to 7 is prepared.
9. a kind of oxygen reduction catalyst that the carbon material being prepared using any the method for claim 1 to 7 is prepared.
10. a kind of activated carbon that the carbon material being prepared using any the method for claim 1 to 7 is prepared.
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