CN108067208A - A kind of renovation process of organic gas adsorption saturation activated carbon - Google Patents
A kind of renovation process of organic gas adsorption saturation activated carbon Download PDFInfo
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- CN108067208A CN108067208A CN201810102312.1A CN201810102312A CN108067208A CN 108067208 A CN108067208 A CN 108067208A CN 201810102312 A CN201810102312 A CN 201810102312A CN 108067208 A CN108067208 A CN 108067208A
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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
- B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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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
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7022—Aliphatic hydrocarbons
- B01D2257/7025—Methane
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7027—Aromatic hydrocarbons
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- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
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Abstract
The present invention provides a kind of renovation process of organic gas adsorption saturation activated carbon, comprise the following steps：1) in protective atmosphere, organic gas adsorption saturation activated carbon is subjected to first step calcining at 200~550 DEG C；2) after the completion of first step calcining, in CO2In atmosphere, second step calcining is carried out at 580~1000 DEG C, obtains regenerated carbon.Result according to the embodiment is understood, using the activated carbon that the invention renovation process obtains after the 5th regeneration cycle its unit adsorbance can still reach after first time regeneration cycle more than 78.65%, the specific surface area after the 5th regeneration cycle can still reach more than 79.8% after first time regeneration cycle.
Description
Technical field
The present invention relates to adsorbent reactivation field more particularly to a kind of regeneration sides of organic gas adsorption saturation activated carbon
Method.
Background technology
Activated carbon is as a kind of common industrial adsorbents, because its internal pore structure is flourishing, specific surface area is very big, absorption
Performance is extremely strong, is suitble to the place used extremely wide etc., is commonly used for adsorbed water body pollutant or gas pollutant.At present, have
Machine gas is a kind of very harmful gas pollutant, because it is with high toxicity, high teratogenesis, high carcinogenic etc., increasingly by
To the concern of researchers.Using many excellent properties of activated carbon, the efficient removal to numerous organic pollutions can be realized, but
Post processing to adsorption saturation activated carbon is still a more stubborn problem.If the activated carbon after adsorption saturation is without place
Reason is i.e. discarded, not only results in the waste of activated carbon resource, will also cause secondary pollution.Therefore, to adsorption saturation activated carbon into
Row regeneration, recovers its absorption property and is reused with realizing, has extremely important engineering application value and economic value.
In the prior art, regenerated for all kinds of adsorption saturation activated carbons, be by changes such as acid, alkali, metal oxides
Microorganisms or the high temperature such as the addition bacterium colony of product are simultaneously realized the methods of apply mobile phase, in retentive activity charcoal
While flourishing pore structure and higher specific surface area, the regenerated carbon of certain performance is obtained.Prepared by these methods
Regenerated carbon, activated carbon can only be regenerated to a certain extent, hydraulic performance decline is very big after regeneration, and operating procedure is numerous
Trivial, reaction condition is complicated, and cost is higher, and industrialized production difficulty is big.
The content of the invention
It is an object of the invention to provide a kind of renovation process of the high organic gas adsorption saturation activated carbon of regeneration efficiency.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The present invention provides a kind of renovation process of organic gas adsorption saturation activated carbon, comprise the following steps：
1) in protective atmosphere, organic gas adsorption saturation activated carbon is subjected to first step calcining at 200~550 DEG C,
Obtain the first calcining materials；
2) in CO2In atmosphere, first calcining materials at 580~1000 DEG C are subjected to second step calcining, are obtained again
Liveliness proof charcoal.
Preferably, in the step 1) in organic gas adsorption saturation activated carbon organic gas for benzene,toluene,xylene,
One or more of formaldehyde, acetic acid, acetone, ether and methane.
Preferably, activated carbon is wood activated charcoal in organic gas adsorption saturation activated carbon in the step 1), coal quality is lived
One or more of property charcoal, active fruit shell carbon and sludge-based activated carbon.
Preferably, providing the protective gas of protective atmosphere in the step 1) includes helium, argon gas or nitrogen；The protection
The flow of gas is 2~10L/min.
Preferably, first step calcining is using room temperature as initial temperature in the step 1), and the first step is risen to through temperature programming
The temperature of calcining, the heating rate of described program heating is 0.5~10 DEG C/min.
Preferably, when the time that the first step is calcined in the step 1) is 0.5~6.5 small.
Preferably, CO in the step 2)2Flow be 0.5~15L/min.
Preferably, in the step 2) second step calcining be using the first step calcining temperature as initial temperature, through program liter
Temperature rises to the temperature of second step calcining, and the heating rate of described program heating is 1~12 DEG C/min.
Preferably, when the time that second step is calcined in the step 2) is 1~10 small.
The present invention provides a kind of renovation process of organic gas adsorption saturation activated carbon, comprise the following steps：1) protecting
It protects in atmosphere, organic gas adsorption saturation activated carbon at 200~550 DEG C is subjected to first step calcining, obtains the first calcined material
Material；2) in CO2In atmosphere, first calcining materials at 580~1000 DEG C are subjected to second step calcining, obtain regeneration activity
Charcoal.The method provided by the invention promotes the thermal decomposition of substance in activated carbon, chemical reaction by calcine by steps well
The adjustment of pore structure in process and activated carbon.Wherein, the first step is calcined, and removes the chemistry in activated carbon at a lower temperature
With reference to water, fugitive constituent, the organic gas adsorbed in activated carbon is promoted to be chemically reacted with activated carbon surface functional group；Second step
Calcining further promotes the chemical reaction between organic gas and activated carbon, and in CO2To activated carbon internal voids knot under effect
Structure is further expanded, and then realizes the high purpose of regeneration efficiency.Result according to the embodiment understands that utilization is of the present invention
The obtained regenerated carbon of renovation process after the 5th regeneration cycle its unit adsorbance can still reach for the first time again
More than 78.65% after raw cycle, the specific surface area after the 5th regeneration cycle can still reach regeneration for the first time and follow
More than 79.8% after ring.
Specific embodiment
The present invention provides a kind of renovation process of organic gas adsorption saturation activated carbon, comprise the following steps：
1) in protective atmosphere, organic gas adsorption saturation activated carbon is subjected to first step calcining at 200~550 DEG C,
Obtain the first calcining materials；
2) in CO2In atmosphere, first calcining materials at 580~1000 DEG C are subjected to second step calcining, are obtained again
Liveliness proof charcoal.
In the present invention, if without specified otherwise, commercially available production that all raw material components are well known to the skilled person
Product.
The present invention carries out the first step at 200~550 DEG C in protective atmosphere, by organic gas adsorption saturation activated carbon and forges
It burns, obtains the first calcining materials；In the present invention, in the organic gas adsorption saturation activated carbon organic gas be preferably benzene,
One or more of toluene, dimethylbenzene, formaldehyde, acetic acid, acetone, ether and methane.In the present invention, when the organic gas
For two or more in above-mentioned specific choice when, the present invention does not have the ratio of each substance special restriction, can be in any proportion
Mixing.
In the present invention, activated carbon is preferably wood activated charcoal, coal quality work in the organic gas adsorption saturation activated carbon
One or more of property charcoal, active fruit shell carbon and sludge-based activated carbon.In the present invention, when the activated carbon is above-mentioned specific
During two or more in selection, the present invention does not have the ratio of each substance special restriction, can mix in any proportion；In this hair
In bright embodiment, cocoanut active charcoal can be selected specifically to.
In the present invention, the temperature of the first step calcining is preferably 250~500 DEG C, more preferably 300~450 DEG C, most
Preferably 350~400 DEG C.In the present invention, when the time of the first step calcining is preferably 0.5~6.5 small, more preferably 2
~6 it is small when, be most preferably 3~5 it is small when.
In the present invention, first step calcining is preferably using room temperature as initial temperature in the step 1), through temperature programming to the
The temperature of one-step calcination；In the present invention, the heating rate of described program heating is preferably 0.5~10 DEG C/min, and more preferably 2
~8 DEG C/min, be most preferably 4~6 DEG C/min.
In the present invention, the protective gas of the protective atmosphere preferably includes helium, argon gas or nitrogen.In the present invention,
The flow of the protective gas is preferably 2~10L/min, more preferably 4~8L/min, is most preferably 5~7L/min.
After obtaining the first calcining materials, the present invention is in CO2In atmosphere, by first calcining materials at 580~1000 DEG C
Lower progress second step calcining, obtains regenerated carbon；In the present invention, the calcining heat is preferably 600~900 DEG C, more excellent
It elects 650~850 DEG C as, is most preferably 700~800 DEG C.In the present invention, it is more excellent when the calcination time is preferably 1~10 small
Elect as 2~8 it is small when, be most preferably 4~6 it is small when.
In the present invention, CO in the step 2)2Gas flow be preferably 0.5~15L/min, more preferably 2~
12L/min is most preferably 5~8L/min.
In the present invention, second step calcining is using the temperature of first step calcining as initial temperature in the step 2), through program
It is warming up to the temperature of second step calcining；In the present invention, the heating rate of described program heating is preferably 1~12 DEG C/min, more
Preferably 2~8 DEG C/min is most preferably 4~6 DEG C/min.
In the present invention, after the completion of second step calcining regenerated carbon is obtained after preferred cooling；The present invention is to the cooling
Process is not particularly limited, and using the type of cooling well-known to those skilled in the art, and achievees the purpose that cooling；It is described
Temperature after cooling is preferably room temperature.
In the present invention, the first step calcining is calcined with second step preferably in the tube furnace with temperature programming function
Middle progress.
The renovation process of organic gas adsorption saturation activated carbon provided by the invention is carried out with reference to embodiment detailed
Explanation, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
The cocoanut active charcoal of 100g benzene vapor adsorption saturations is placed in the tube furnace with temperature programming function, in Ar atmosphere
Under, Ar gas flows is controlled, using room temperature as initial temperature, 330 DEG C to be warming up to simultaneously with the heating rate of 6.2 DEG C/min for 5L/min
Constant temperature is kept, 4.5h is calcined, obtains the first calcining materials；
In CO2Under atmosphere, CO is controlled2Gas flow is 3.4L/min, with 330 DEG C for initial temperature, with 5.8 DEG C/min's
Heating rate is warming up to 720 DEG C and keeps constant temperature, and first calcining materials are calcined 6.1h, is cooled to room temperature, obtains
Regenerated carbon.
According to national standard GB 2890-2009《Respiratory protection self-absorbing filtering type gas defence mask》In relevant regulations, described in test
Regenerated carbon is to the absorption property of benzene, and after first time regeneration cycle, unit adsorbance is 358.2mg/g, and specific surface area is
1225.89m2/g；After third time regeneration cycle, unit adsorbance is 326.10mg/g, specific surface area 1127.55m2/g；The
After five regeneration cycles, unit adsorbance is 281.72mg/g, specific surface area 1008.53m2/g。
Embodiment 2
The cocoanut active charcoal of 2000g benzene vapor adsorption saturations is placed in the tube furnace with temperature programming function, in He gas
Under atmosphere, He gas flows is controlled, using room temperature as initial temperature, 380 DEG C to be warming up to the heating rate of 7 DEG C/min for 4.2L/min
And constant temperature is kept, 5.5h is calcined, obtains the first calcining materials；
In CO2Under atmosphere, CO is controlled2Gas flow is 3.5L/min, with 330 DEG C for initial temperature, with 4.5 DEG C/min's
Heating rate is warming up to 820 DEG C and keeps constant temperature, and first calcining materials are calcined 7h, is cooled to room temperature, obtains again
Liveliness proof charcoal.
According to national standard GB 2890-2009《Respiratory protection self-absorbing filtering type gas defence mask》In relevant regulations, test the work
Property charcoal to the absorption property of benzene, after first time regeneration cycle, unit adsorbance is 320.62mg/g, and specific surface area is
1127.79m2/g；After third time regeneration cycle, unit adsorbance is 304.20mg/g, specific surface area 1020.35m2/g；The
After five regeneration cycles, unit adsorbance is 279.19mg/g, specific surface area 900.10m2/g。
Embodiment 3
The cocoanut active charcoal of 4000g benzene vapor adsorption saturations is placed in the tube furnace with temperature programming function, in N2Gas
Under atmosphere, N is controlled2Gas flow is 6L/min, and using room temperature as initial temperature, 350 DEG C are warming up to simultaneously with the heating rate of 5 DEG C/min
Constant temperature is kept, 4h is calcined, obtains the first calcining materials；
After the completion of first step calcining, in CO2Under atmosphere, CO is controlled2Gas flow is 2.5L/min, is starting temperature with 350 DEG C
Degree, is warming up to 750 DEG C with the heating rate of 6.5 DEG C/min and keeps constant temperature, and first calcining materials are calcined 5h, cold
But to room temperature, the activated carbon after being regenerated.
According to national standard GB 2890-2009《Respiratory protection self-absorbing filtering type gas defence mask》In relevant regulations, test the work
Property charcoal to the absorption property of benzene, after first time regeneration cycle, unit adsorbance is 338.50mg/g, and specific surface area is
1199.65m2/g；After third time regeneration cycle, unit adsorbance is 310.37mg/g, specific surface area 1050.20m2/g；The
After five regeneration cycles, unit adsorbance is 278.69mg/g, specific surface area 1000.27m2/g。
Comparative example 1
By the cocoanut active charcoal of 100g benzene vapor adsorption saturations be placed in 10% hydrochloric acid solution submergence 3 it is small when, shaking
It when mixing 7 is small on bed, is then boiled 30 minutes in electric furnace, it is neutral, drying to be rinsed repeatedly with deionized water to pH value；
28~32 mesh are ground in grinder, are put into regenerative response kettle, with supercritical CO2To regenerate atmosphere, super
Critical CO2Flow is 1mL/min, and regeneration kettle pressure is 16MPa, when temperature is that processing 2 is small at 45 DEG C, is then subtracted through pressure reducing valve
Pressure, absorbing liquid absorption handle to obtain regenerated carbon.
According to national standard GB 2890-2009《Respiratory protection self-absorbing filtering type gas defence mask》In relevant regulations, test the work
Property charcoal to the absorption property of benzene, after five regenerative processes, the adsorbance of the regenerated carbon is the 68% of former activated carbon.
As seen from the above embodiment, the present invention provides a kind of renovation process of organic gas adsorption saturation activated carbon, profits
With the regenerated carbon that renovation process of the present invention obtains, its unit adsorbance still can be with after the 5th regeneration cycle
Reach more than 78.65% after first time regeneration cycle, the specific surface area after the 5th regeneration cycle can still reach
More than 79.8% after first time regeneration cycle.Five regenerative processes of regeneration method of active carbon more commonly used in the prior art it
Adsorbance afterwards has higher regenerability for the 68% of former activated carbon.
The above is only the preferred embodiment of the present invention, not makees limitation in any form to the present invention.It should
It points out, for those skilled in the art, without departing from the principle of the present invention, if can also make
Dry improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of renovation process of organic gas adsorption saturation activated carbon, comprises the following steps：
1) in protective atmosphere, organic gas adsorption saturation activated carbon at 200~550 DEG C is subjected to first step calcining, is obtained
First calcining materials；
2) in CO2In atmosphere, first calcining materials at 580~1000 DEG C are subjected to second step calcining, obtain regeneration activity
Charcoal.
2. renovation process as described in claim 1, which is characterized in that organic gas adsorption saturation activated carbon in the step 1)
Middle organic gas is one or more of benzene,toluene,xylene, formaldehyde, acetic acid, acetone, ether and methane.
3. renovation process as claimed in claim 1 or 2, which is characterized in that organic gas adsorption saturation is lived in the step 1)
Property charcoal in activated carbon one or more of for wood activated charcoal, coaly activated carbon, active fruit shell carbon and sludge-based activated carbon.
4. renovation process as described in claim 1, which is characterized in that the protective gas of protective atmosphere in the step 1) is provided
Including helium, argon gas or nitrogen；The flow of the protective gas is 2~10L/min.
5. renovation process as described in claim 1, which is characterized in that in the step 1) first step calcining be using room temperature for
Beginning temperature rises to the temperature of first step calcining through temperature programming, and the heating rate of described program heating is 0.5~10 DEG C/min.
6. the renovation process as described in claim 1 or 5, which is characterized in that the time of first step calcining is in the step 1)
0.5~6.5 it is small when.
7. renovation process as described in claim 1, which is characterized in that CO in the step 2)2Flow be 0.5~15L/
min。
8. renovation process as described in claim 1, which is characterized in that second step calcining is forged with the first step in the step 2)
The temperature of burning is initial temperature, rises to the temperature of second step calcining through temperature programming, the heating rate of described program heating for 1~
12℃/min。
9. the renovation process as described in claim 1 or 8, which is characterized in that the time that second step is calcined in the step 2) is 1
~10 it is small when.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111921513A (en) * | 2020-08-31 | 2020-11-13 | 天津市环境保护科学研究院 | Saturated activated carbon regeneration treatment device and method for absorbing VOCs gas |
| CN113731120A (en) * | 2021-09-22 | 2021-12-03 | 河南佳诺威木业有限公司 | MDF tail gas standard emission process |
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Cited By (3)
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| CN111921513A (en) * | 2020-08-31 | 2020-11-13 | 天津市环境保护科学研究院 | Saturated activated carbon regeneration treatment device and method for absorbing VOCs gas |
| CN113731120A (en) * | 2021-09-22 | 2021-12-03 | 河南佳诺威木业有限公司 | MDF tail gas standard emission process |
| CN113731120B (en) * | 2021-09-22 | 2024-03-26 | 河南佳诺威木业有限公司 | MDF tail gas standard emission process |
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Application publication date: 20180525 |