CN106732485A - A kind of method of cobalt based compound catalytic regeneration activated carbon - Google Patents
A kind of method of cobalt based compound catalytic regeneration activated carbon Download PDFInfo
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- CN106732485A CN106732485A CN201610997577.3A CN201610997577A CN106732485A CN 106732485 A CN106732485 A CN 106732485A CN 201610997577 A CN201610997577 A CN 201610997577A CN 106732485 A CN106732485 A CN 106732485A
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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
- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
Abstract
The invention discloses a kind of method of cobalt based compound catalytic regeneration activated carbon, comprise the following steps：Step (1)：Activated carbon to be regenerated, cobalt series catalyst are dispersed in water to obtain slurries, then the hydro-thermal reaction under 230~280 DEG C, 28~64atm；Described cobalt series catalyst is the simple substance and/or oxide of cobalt；Step (2)：With the hydro-thermal reaction liquid of acid dilution step (1), regenerated carbon is obtained through ultrasound, separation of solid and liquid, dried process after.Organic matter fast reaction of the present invention by superheated water under the catalytic action of cobalt metal simple-substance or the compound of cobalt with absorption in waste active carbon, macromolecular is decomposed into small organic molecule, is even decomposed into CO2And water, by being cleaned by ultrasonic activated carbon hole in residue reach regeneration purpose.
Description
Technical field
The invention belongs to the regeneration field that saturation adsorbs organic matter activated carbon, and in particular to one kind is made using cobalt based compound
For catalyst carries out regeneration method by hydro-thermal reaction to activated carbon.
Background technology
Regenerating active carbon refers on the premise of activated carbon original structure is not destroyed, with either physically or chemically removal absorption
In the adsorbate of activated carbon capillary, recover the process of its absorption property.Current regeneration method of active carbon mainly has ultrasonic regeneration
Method, electrochemical regeneration method, super face fluid method of reproduction, solvent regeneration process, oxidation reclaiming process, hot recycling method, bio-regeneration method etc..It is logical
Often, existing regeneration method of active carbon has the following disadvantages：1. activated carbon loss is larger；2. adsorption capacity has substantially after regenerating
Decline；The tail gas produced when 3. regenerating can cause secondary pollution；4. regeneration condition is harsh, and exploitativeness difficulty is larger, cost
With higher, economic benefit is low.
The Chinese patent literature of Publication No. CN102989435 A discloses a kind of method of regenerating active carbon, its feature
It is main including well mixed toward addition acid in inactivation activated carbon, activated carbon is placed in thermal regeneration in vacuum heater；
The Chinese patent literature of Publication No. CN105582904 A discloses a kind of renovation process of activated carbon, its feature
It is that the main regenerated solvent for including being made up of alkaline matter, organic solvent and water and waste active carbon are carried out according to certain volume ratio
Mixing, the Pre-Treatment of Activated charcoal after then microwave is to washing is activated；
The Chinese patent literature of Publication No. CN105080521 A discloses a kind of renovation process of activated carbon, main logical
Cross desorption liquid (organic solvent and water) and mix with activated carbon and be beaten to obtain slurry, the slurry is post-treated to obtain regenerated carbon, take off
Attached liquid carries out catalytic treatment by one or more catalyst of mantoquita, rhodium salt and palladium salt, reaches the purpose of recycling.The party
Method need in advance add organic solvent, and by similar compatibility principle by the organic matter dissolution in activated carbon, then wet oxidation is dropped again
The organic matter of dissolution is solved, regenerating active carbon purpose is reached；DMF and DMSO high costs that the present invention is added and easily environment is made
Into secondary pollution；The present invention also indicates that do not add the regenerating active carbon poor effect of described organic solvent, loss late is up to
18%, regeneration rate is only 25%.
Current active carbon regenerating technology main flow is high temperature regeneration, solvent reclamation, and high temperature regeneration cannot then avoid high energy consumption
Problem, solvent reclamation easily brings organic solvent secondary pollution problems.Therefore be badly in need of provide one kind can reducing energy consumption, again need
Avoid the regeneration techniques of organic solvent secondary pollution.
The content of the invention
Need to add a large amount of organic solvents, treatment conditions harshness, regeneration effect difference etc. to solve existing regenerating active carbon and ask
Topic, regeneration method is carried out the invention provides one kind by hydro-thermal reaction as catalyst using cobalt system's material to activated carbon；
It is intended to reduce carbon depletion, the absorption property of the activated carbon that lifting regeneration is obtained.
Big quantity of material (such as organic matter) is adsorbed with the microscopic voids of activated carbon (waste active carbon) to be regenerated, especially
Large amount of complex macromolecule, the waste active carbon of the macromolecule organic of bulky grain are adsorbed with, its pore plugging is serious, and intractability is remote
More than homogeneous system, though high temperature, high pressure contribute to the treatment of activated carbon organic matter, the structure of activated carbon, carbon loss are easily destroyed
Consumption is high；Seek mild condition, the key of efficient Regenevating Waste Activated Carbon method always waste active carbon process field.
The present inventor is attempted using metallic compounds such as mantoquita, palladium salts as catalyst, and activated carbon to be regenerated is carried out
Hydro-thermal reaction, but carbon depletion it is higher and regeneration after activated carbon absorption property it is low.By further exploration discovery, use
Cobalt system material can effectively reduce the loss of activated carbon and lift its absorption property, but still be difficult to reach ideal effect.By depth
Enter research, it is a discovery of the invention that unexpected by controlling to be can reach in specific scope the temperature and pressure of hydro-thermal reaction
Regeneration effect, the classification of waste active carbon applicatory is wide, is especially adsorbed with the useless of macromolecule organic or bulky grain organic matter
The regeneration of activated carbon；Therefore following technical scheme is provided：
A kind of method of cobalt based compound catalytic regeneration activated carbon, comprises the following steps：
Step (1)：Activated carbon to be regenerated, cobalt series catalyst are dispersed in water to obtain slurries, then 230~280 DEG C,
Hydro-thermal reaction under 28~64atm；Described cobalt series catalyst is the simple substance and/or oxide of cobalt；
Step (2)：With the hydro-thermal reaction liquid of acid dilution step (1), obtained through ultrasound, separation of solid and liquid, dried process after
Regenerated carbon.
In the present invention, under the catalysis of cobalt series catalyst, and coordinate the temperature and pressure of described hydro-thermal reaction, water transformation
Into the superheated water of mass efficient activity, and then can efficiently change or react to be regenerated on the premise of without organic solvent
The organic matter of activated carbon, small molecule even CO is decomposed into by organic macromolecule2And water, then it is cleaned by ultrasonic in acid condition again
Residue in activated carbon hole, so as to reach the purpose of efficient, the gentle regeneration of waste active carbon.In the present invention, regeneration condition temperature
With, the microstructure of activated carbon can be efficiently dredged, the porosity of activated carbon is expanded, reduce the loss of activated carbon.
Preferably, in step (1), described cobalt series catalyst is Co, CoO, Co2O3In at least one.
The inventors discovered that, using the simple substance and oxide catalyst of described cobalt under, hydro-thermal reaction can be in a mild condition
Carry out, help to lift the performance of regenerated carbon.
Further preferably, in step (1), described cobalt series catalyst is Co2O3。
Coordinate described cobalt series catalyst, the pressure of preferred hydro-thermal reaction is 40~64atm；Most preferably 46~
55atm。
Under the preferred pressure, the temperature of preferred hydro-thermal reaction is 250~280 DEG C；Most preferably 260~
270℃。
Preferably, described activated carbon to be regenerated is washed through deionized water in advance.
In the present invention, activated carbon to be regenerated carries out washing pretreatment using deionized water in advance before step (1) is carried out,
For removing the acidic materials in waste active carbon and part soluble inorganic matter, the catalysis for further improving catalyst is contributed to imitate
Really.
Preferably, in step (1), the dosage of described cobalt series catalyst is activated carbon weight to be regenerated
0.1%~5%；More preferably 1%~3wt%.
In the present invention, the hydro-thermal reaction time is 1~5h；It is preferably 2~3h.
In the present invention, the activated carbon to be regenerated and cobalt series catalyst of the part by weight are dispersed in water, stirred
Obtain slurries.Preferably, in step (1), in described slurries, liquid/solid weight ratio is 10: 1~2: 1.
Described liquid/solid weight is than the activated carbon and the gross weight and the weight ratio of water of cobalt series catalyst in finger slurries.
Preferably, in step (1), in described slurries, the gross weight and water of activated carbon to be regenerated and cobalt series catalyst
Weight be 2~10: 1；Preferably 6~8：1.
Preferably, in step (2), described acid solution is the aqueous solution of inorganic acid, concentration expressed in percentage by weight is 1~
10%.
Further preferably, described inorganic acid is, for example, hydrochloric acid.
The concentration of described acid solution is 2~5%.
It is 30~20: 1 to use described acid solution that hydro-thermal reaction liquid is diluted into liquid/solid weight ratio.
Then the dilution to acid solution carries out supersound washing, preferably, in step (2), ultrasonically treated frequency is
20KHz~23KHz.
Supersound washing 2~4 times under described ultrasound condition, every time wash 30~40min, then filtering, air-dry obtain
Regenerated carbon.
A kind of preferred regeneration method of active carbon of the present invention, comprises the following steps：
Step (a)：Waste active carbon is washed with deionized 2~3 times；Activated carbon after the cleaning being then filtrated to get,
Step (b)：Step (a) is obtained activated carbon and cobalt series catalyst (dosage for activated carbon weight 0.1%~
5%) it is added in hydrothermal synthesis reaction kettle for 10: 1~2: 1 ratio is well mixed with deionized water according to liquid/solid ratio,
Under 28~64atm pressure, reacted 1~5 hour at a temperature of 230~280 DEG C, be then cooled to taking-up hydro-thermal at less than 50 DEG C anti-
Answer liquid；Described cobalt series catalyst is selected from Co, CoO and Co2O3In at least one；
Step (c)：It is 30~20: 1 that hydro-thermal reaction liquid is diluted into liquid/solid ratio with 2~5% watery hydrochloric acid, is placed in ultrasound
Washed under 20KHz~23KHz in concussion washer 2~4 times, 30~40min is washed every time, in separation of solid and liquid, dry again
Liveliness proof charcoal.
The beneficial effects of the present invention are：
In the present invention, under described cobalt series catalyst catalysis, and coordinate the parameters such as described pressure and temperature, body can be made
Form a large amount of superheated waters in system, so reach without additionally addition organic solvent, it is gentle under conditions of be capable of achieving it is useless active
The highly efficient regeneration of charcoal.Below 300 DEG C, the charcoal of regenerated carbon damages smaller to treatment temperature of the invention；Under the described conditions,
Larger molecular organicses in activated carbon can rapidly be decomposed into small organic molecule, CO2And water, and coordinate ultrasonic vibration washing, can
Effectively dredging activated carbon hole, recovers absorption property, reaches regeneration purpose.In the present invention, regenerated carbon quality is good, charcoal is damaged
It is low, remain to keep preferable absorption property after the multiple circular regeneration of activated carbon, the recovery time is short, efficiency high, greatly reduces energy
Consumption, with very big economic benefit.
In the present invention, the charcoal of regenerated carbon is damaged and can be down to 2.2%, and absorption property can match in excellence or beauty new charcoal.
Specific embodiment
With reference to embodiment, the present invention is described in detail.If it should be noted that not conflicting, the present invention is implemented
Each feature in example and embodiment can be combined with each other, within protection scope of the present invention.
Following examples and comparative example, the activated carbon for the treatment of take from the useless activity after domestic certain enterprise's Industrial Wastewater Treatment
Charcoal, is adsorbed with macromolecule organic and bulky grain organic matter, such as contains phenols, alcohol, benzene and its derivative.Described useless activity is right
Iodine and methylene blue are substantially without adsorption effect.
Embodiment 1
The renovation process of activated carbon is mainly included the following steps that：
Step (1)：Waste active carbon is washed with deionized 2~3 times, removes the soluble nothing of acidic materials therein and part
Machine thing, prevents it from side reaction occurring with catalyst and catalytic effect is influenceed, and filter, separate；
Step (2)：Step (1) is separated by filtration the activated carbon for obtaining, with mass ratio 0.5% (with activated carbon weight as base
It is accurate) allocate Co into2O3As catalyst, according to liquid-solid ratio for 2: 1 ratio is well mixed with deionized water, polyparaphenylene is added to
In hydrothermal synthesis reaction kettle, 230 DEG C are heated to, air pressure is 28atm, heat-insulation pressure keeping 1h, carry out organic matter decomposition, dissolution reaction,
Slurry (hydro-thermal reaction liquid) is taken out when being cooled to less than 50 DEG C；
Step (3)：It is 30~20: 1 that slurry is diluted into liquid-solid ratio with 5% watery hydrochloric acid, is placed in ultrasonic vibration washer
Middle is that 20KHz~23KHz carries out 30~40min of washing with frequency, is repeated 2~4 times, fully washes away catalyst impurities and activated carbon
Residue in hole, dries and can obtain regenerated carbon naturally.
The regenerated carbon obtained by above-mentioned steps carries out absorption property, charcoal to be damaged carries out the new activated carbon of test comparison, obtains
Go out iodine sorption value returns to new charcoal 93%, methylene blue adsorption value returns to the 88% of new charcoal, charcoal damages 2.2%, and charcoal damages relatively low,
Regenerative adsorption performance can be satisfied by general regeneration requirements.
Embodiment 2
The renovation process of activated carbon is mainly included the following steps that：
Step (1)：Waste active carbon is washed with deionized 2~3 times, removes the soluble nothing of acidic materials therein and part
Machine thing, prevents it from side reaction occurring with catalyst and catalytic effect is influenceed, and filter, separate；
Step (2)：Step (1) is separated by filtration the activated carbon for obtaining, by mass ratio 1% (on the basis of activated carbon weight)
Allocate Co into2O3As catalyst, according to liquid-solid ratio for 6: 1 ratio is well mixed with deionized water, polyparaphenylene hydro-thermal is added to
In synthesis reaction vessel, 250 DEG C are heated to, air pressure is 40atm, heat-insulation pressure keeping 3h, carry out organic matter decomposition, dissolution reaction, cooling
To taking-up slurry (hydro-thermal reaction liquid) at less than 50 DEG C；
Step (3)：It is 30~20: 1 that slurry is diluted into liquid-solid ratio with 5% watery hydrochloric acid, is placed in ultrasonic vibration washer
Middle is that 20KHz~23KHz carries out 30~40min of washing with frequency, is repeated 2~4 times, fully washes away catalyst impurities and activated carbon
Residue in hole, dries and can obtain regenerated carbon naturally.
The regenerated carbon obtained by above-mentioned steps carries out absorption property, charcoal to be damaged carries out the new activated carbon of test comparison, obtains
Go out iodine sorption value returns to new charcoal 97%, methylene blue adsorption value returns to the 93% of new charcoal, charcoal damages 3%, and charcoal damages moderate, then
Raw absorption property can be satisfied by general regeneration requirements.
Embodiment 3
The renovation process of activated carbon is mainly included the following steps that：
Step (1)：Waste active carbon is washed with deionized 2~3 times, removes the soluble nothing of acidic materials therein and part
Machine thing, prevents it from side reaction occurring with catalyst and catalytic effect is influenceed, and filter, separate；
Step (2)：Step (1) is separated by filtration the activated carbon for obtaining, by mass ratio 2% (on the basis of activated carbon weight)
Allocate Co into2O3As catalyst, according to liquid-solid ratio for 8: 1 ratio is well mixed with deionized water, polyparaphenylene hydro-thermal is added to
In synthesis reaction vessel, 260 DEG C are heated to, air pressure is 47atm, heat-insulation pressure keeping 3h, carry out organic matter decomposition, dissolution reaction, cooling
To taking-up slurry (hydro-thermal reaction liquid) at less than 50 DEG C；
Step (3)：It is 30~20: 1 that slurry is diluted into liquid-solid ratio with 5% watery hydrochloric acid, is placed in ultrasonic vibration washer
Middle is that 20KHz~23KHz carries out 30~40min of washing with frequency, is repeated 2~4 times, fully washes away catalyst impurities and activated carbon
Residue in hole, dries and can obtain regenerated carbon naturally.
The regenerated carbon obtained by above-mentioned steps carries out absorption property, charcoal to be damaged carries out the new activated carbon of test comparison, obtains
Go out iodine sorption value returns to new charcoal 103%, methylene blue adsorption value returns to the 96% of new charcoal, charcoal damages 3.2%, and charcoal damages suitable
In, various aspects of performance is satisfied by regeneration requirements.
Embodiment 4
The renovation process of activated carbon is mainly included the following steps that：
Step (1)：Waste active carbon is washed with deionized 2~3 times, removes the soluble nothing of acidic materials therein and part
Machine thing, prevents it from side reaction occurring with catalyst and catalytic effect is influenceed, and filter, separate；
Step (2)：By step (1)：The activated carbon for obtaining is separated by filtration, with mass ratio 5% (with activated carbon weight as base
It is accurate) allocate Co into2O3As catalyst, according to liquid-solid ratio for 10: 1 ratio is well mixed with deionized water, polyparaphenylene is added to
In hydrothermal synthesis reaction kettle, 280 DEG C are heated to, air pressure is 64atm, heat-insulation pressure keeping 5h, carry out organic matter decomposition, dissolution reaction,
Slurry (hydro-thermal reaction liquid) is taken out when being cooled to less than 50 DEG C；
Step (3)：It is 30~20: 1 that slurry is diluted into liquid-solid ratio with 5% watery hydrochloric acid, is placed in ultrasonic vibration washer
Middle is that 20KHz~23KHz carries out 30~40min of washing with frequency, is repeated 2~4 times, fully washes away catalyst impurities and activated carbon
Residue in hole, dries and can obtain regenerated carbon naturally.
The regenerated carbon obtained by above-mentioned steps carries out absorption property, charcoal to be damaged carries out the new activated carbon of test comparison, obtains
Go out iodine sorption value returns to new charcoal 110%, methylene blue adsorption value returns to the 108% of new charcoal, charcoal damages 5.3%, and charcoal was damaged
Greatly, absorption property is preferable.
Embodiment 5
The renovation process of activated carbon is mainly included the following steps that：
Step (1)：Waste active carbon is washed with deionized 2~3 times, removes the soluble nothing of acidic materials therein and part
Machine thing, prevents it from side reaction occurring with catalyst and catalytic effect is influenceed, and filter, separate；
Step (2)：By step (1)：The activated carbon for obtaining is separated by filtration, with mass ratio 3% (with activated carbon weight as base
It is accurate) allocate Co into2O3As catalyst, according to liquid-solid ratio for 10: 1 ratio is well mixed with deionized water, polyparaphenylene is added to
In hydrothermal synthesis reaction kettle, 280 DEG C are heated to, air pressure is 64atm, heat-insulation pressure keeping 3h, carry out organic matter decomposition, dissolution reaction,
Slurry (hydro-thermal reaction liquid) is taken out when being cooled to less than 50 DEG C；
Step (3)：It is 30~20: 1 that slurry is diluted into liquid-solid ratio with 5% watery hydrochloric acid, is placed in ultrasonic vibration washer
Middle is that 20KHz~23KHz carries out 30~40min of washing with frequency, is repeated 2~4 times, fully washes away catalyst impurities and activated carbon
Residue in hole, dries and can obtain regenerated carbon naturally.
The regenerated carbon obtained by above-mentioned steps carries out absorption property, charcoal to be damaged carries out the new activated carbon of test comparison, obtains
Go out iodine sorption value returns to new charcoal 118%, methylene blue adsorption value returns to the 107% of new charcoal, charcoal damages 4.5%, and charcoal is damaged slightly
Height, regenerative adsorption excellent performance.
Embodiment 6
The renovation process of activated carbon is mainly included the following steps that：
Step (1)：Waste active carbon is washed with deionized 2~3 times, removes the soluble nothing of acidic materials therein and part
Machine thing, prevents it from side reaction occurring with catalyst and catalytic effect is influenceed, and filter, separate；
Step (2)：By step (1)：The activated carbon for obtaining is separated by filtration, with mass ratio 2% (with activated carbon weight as base
It is accurate) allocate Co into2O3As catalyst, according to liquid-solid ratio for 8: 1 ratio is well mixed with deionized water, polyparaphenylene is added to
In hydrothermal synthesis reaction kettle, 270 DEG C are heated to, air pressure is 55atm, heat-insulation pressure keeping 3h, carry out organic matter decomposition, dissolution reaction,
Slurry (hydro-thermal reaction liquid) is taken out when being cooled to less than 50 DEG C；
Step (3)：It is 30~20: 1 that slurry is diluted into liquid-solid ratio with 5% watery hydrochloric acid, is placed in ultrasonic vibration washer
Middle is that 20KHz~23KHz carries out 30~40min of washing with frequency, is repeated 2~4 times, fully washes away catalyst impurities and activated carbon
Residue in hole, dries and can obtain regenerated carbon naturally.
The regenerated carbon obtained by above-mentioned steps carries out absorption property, charcoal to be damaged carries out the new activated carbon of test comparison, obtains
Go out iodine sorption value returns to new charcoal 116%, methylene blue adsorption value returns to the 104% of new charcoal, charcoal damages 3.5%, and charcoal damages suitable
In, regenerative adsorption excellent performance.
Comparative example 1
The renovation process of activated carbon is mainly included the following steps that：
Step (1)：Waste active carbon is washed with deionized 2~3 times, removes the soluble nothing of acidic materials therein and part
Machine thing, prevents it from side reaction occurring with catalyst and catalytic effect is influenceed, and filter, separate；
Step (2)：By step (1)：The activated carbon for obtaining is separated by filtration, with mass ratio 2% (with activated carbon weight as base
It is accurate) CuSO4 is allocated into as catalyst, according to liquid-solid ratio for 8: 1 ratio is well mixed with deionized water, it is added to polyparaphenylene
In hydrothermal synthesis reaction kettle, 280 DEG C are heated to, air pressure is 64atm, heat-insulation pressure keeping 5h, carry out organic matter decomposition, dissolution reaction,
Slurry (hydro-thermal reaction liquid) is taken out when being cooled to less than 50 DEG C；
Step (3)：It is 30~20: 1 that slurry is diluted into liquid-solid ratio with 5% watery hydrochloric acid, is placed in ultrasonic vibration washer
Middle is that 20KHz~23KHz carries out 30~40min of washing with frequency, is repeated 2~4 times, fully washes away catalyst impurities and activated carbon
Residue in hole, dries and can obtain regenerated carbon naturally.
The regenerated carbon obtained by above-mentioned steps carries out absorption property, charcoal to be damaged carries out the new activated carbon of test comparison, obtains
Go out iodine sorption value returns to new charcoal 73%, methylene blue adsorption value returns to the 65% of new charcoal, charcoal damages 1.3%, charcoal damage it is low but
It is that absorption property fails to reach regeneration requirements.
Comparative example 2
The renovation process of activated carbon is mainly included the following steps that：
Step (1)：Waste active carbon is washed with deionized 2~3 times, removes the soluble nothing of acidic materials therein and part
Machine thing, prevents it from side reaction occurring with catalyst and catalytic effect is influenceed, and filter, separate；
Step (2)：By step (1)：The activated carbon for obtaining is separated by filtration, (is with activated carbon weight with mass ratio 0.05%
Benchmark) allocate Co into2O3As catalyst, according to liquid-solid ratio for 8: 1 ratio is well mixed with deionized water, contraposition is added to poly-
In benzene hydrothermal synthesis reaction kettle, 200 DEG C are heated to, air pressure is 15atm, heat-insulation pressure keeping 3h, carry out organic matter decomposition, dissolution anti-
Should, take out slurry (hydro-thermal reaction liquid) when being cooled to less than 50 DEG C；
Step (3)：It is 30~20: 1 that slurry is diluted into liquid-solid ratio with 5% watery hydrochloric acid, is placed in ultrasonic vibration washer
Middle is that 20KHz~23KHz carries out 30~40min of washing with frequency, is repeated 2~4 times, fully washes away catalyst impurities and activated carbon
Residue in hole, dries and can obtain regenerated carbon naturally.
The regenerated carbon obtained by above-mentioned steps carries out absorption property, charcoal to be damaged carries out the new activated carbon of test comparison, obtains
Go out iodine sorption value returns to new charcoal 73%, methylene blue adsorption value returns to the 62% of new charcoal, charcoal damages 1.5%, and charcoal damages relatively low
But absorption property fails to reach regeneration requirements.
Comparative example 3
The renovation process of activated carbon is mainly included the following steps that：
Step (1)：Waste active carbon is washed with deionized 2~3 times, removes the soluble nothing of acidic materials therein and part
Machine thing, prevents it from side reaction occurring with catalyst and catalytic effect is influenceed, and filter, separate；
Step (2)：By step (1)：The activated carbon for obtaining is separated by filtration, with mass ratio 2% (with activated carbon weight as base
It is accurate) allocate Co into2O3As catalyst, according to liquid-solid ratio for 8: 1 ratio is well mixed with deionized water, polyparaphenylene is added to
In hydrothermal synthesis reaction kettle, 270 DEG C are heated to, air pressure is 55atm, heat-insulation pressure keeping 3h, carry out organic matter decomposition, dissolution reaction,
Material is taken out when being cooled to less than 50 DEG C, is dried naturally and be can obtain regenerated carbon.
The regenerated carbon obtained by above-mentioned steps carries out absorption property, charcoal to be damaged carries out the new activated carbon of test comparison, obtains
Go out iodine sorption value returns to new charcoal 86%, methylene blue adsorption value returns to the 74% of new charcoal, charcoal damages 1.7%, and charcoal damages relatively low
But absorption property fails to reach regeneration requirements.
Comparative example 4
According to the optimal renovation process of activated carbon of the Chinese patent of Publication No. CN105080521 A, to institute in this patent
The waste active carbon for the treatment of is regenerated, and the regenerated carbon for obtaining carries out absorption property, charcoal to be damaged carries out the new activated carbon of test comparison,
Show that iodine sorption value returns to the 81% of new charcoal, methylene blue adsorption value returns to the 64% of new charcoal, and charcoal damages 2.7%, and charcoal damages low
But absorption property fails to reach regeneration requirements.
Claims (10)
1. a kind of method of cobalt based compound catalytic regeneration activated carbon, it is characterised in that comprise the following steps：
Step (1)：Activated carbon to be regenerated, cobalt series catalyst are dispersed in water to obtain slurries, then 230~280 DEG C, 28~
Hydro-thermal reaction under 64atm；Described cobalt series catalyst is the simple substance and/or oxide of cobalt；
Step (2)：With the hydro-thermal reaction liquid of acid dilution step (1), must be regenerated through ultrasound, separation of solid and liquid, dried process after
Activated carbon.
2. the method for cobalt based compound catalytic regeneration activated carbon as claimed in claim 1, it is characterised in that in step (1), institute
The cobalt series catalyst stated is Co, CoO, Co2O3In at least one.
3. the method for cobalt based compound catalytic regeneration activated carbon as claimed in claim 1, it is characterised in that in step (1), institute
The cobalt series catalyst stated is Co2O3。
4. the method for cobalt based compound catalytic regeneration activated carbon as claimed in claim 2, it is characterised in that in step (1), institute
The dosage of the cobalt series catalyst stated is the 0.1%~5% of activated carbon weight to be regenerated.
5. the method for the cobalt based compound catalytic regeneration activated carbon as described in Claims 1 to 4, it is characterised in that hydro-thermal reaction
Pressure be 40~64atm.
6. the method for cobalt based compound catalytic regeneration activated carbon as claimed in claim 5, it is characterised in that the temperature of hydro-thermal reaction
Spend is 250~280 DEG C.
7. the method for cobalt based compound catalytic regeneration activated carbon as claimed in claim 6, it is characterised in that the hydro-thermal reaction time
It is 1~5h.
8. the method for cobalt based compound catalytic regeneration activated carbon as claimed in claim 7, it is characterised in that in step (1), institute
In the slurries stated, liquid/solid weight ratio is 10: 1~2: 1.
9. the method for cobalt based compound catalytic regeneration activated carbon as claimed in claim 8, it is characterised in that in step (2), institute
The acid solution stated is the aqueous solution of inorganic acid, and concentration expressed in percentage by weight is 1~10%；It is using described acid solution that hydro-thermal reaction liquid is dilute
It is 30~20: 1 to release to liquid/solid weight ratio.
10. the method for cobalt based compound catalytic regeneration activated carbon as claimed in claim 9, it is characterised in that in step (2),
Ultrasonically treated frequency is 20KHz~23KHz.
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| CN109433172A (en) * | 2018-10-23 | 2019-03-08 | 上海大学 | The regeneration treating method of Alveolate activated carbon |
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| CN1370618A (en) * | 2000-12-05 | 2002-09-25 | Zeo技术公司 | Oxidizing catalyst and its preparation, regeneration process and usage in treating waste water |
| CN1462729A (en) * | 2003-06-19 | 2003-12-24 | 上海交通大学 | Treatment process for two stage recycling alkali waste liquid drained off by process system of synthesizing octanol |
| EP1410844A1 (en) * | 2002-10-15 | 2004-04-21 | Centre National De La Recherche Scientifique (Cnrs) | Silicon-based porous catalytic system for oligomerising light olefins |
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| CN1370618A (en) * | 2000-12-05 | 2002-09-25 | Zeo技术公司 | Oxidizing catalyst and its preparation, regeneration process and usage in treating waste water |
| EP1410844A1 (en) * | 2002-10-15 | 2004-04-21 | Centre National De La Recherche Scientifique (Cnrs) | Silicon-based porous catalytic system for oligomerising light olefins |
| CN1462729A (en) * | 2003-06-19 | 2003-12-24 | 上海交通大学 | Treatment process for two stage recycling alkali waste liquid drained off by process system of synthesizing octanol |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109433172A (en) * | 2018-10-23 | 2019-03-08 | 上海大学 | The regeneration treating method of Alveolate activated carbon |
| CN109433172B (en) * | 2018-10-23 | 2022-01-07 | 上海大学 | Regeneration treatment method of honeycomb activated carbon |
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