CN109437189A - A kind of preparation of resin based sphere active carbon and application method - Google Patents
A kind of preparation of resin based sphere active carbon and application method Download PDFInfo
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- CN109437189A CN109437189A CN201811534882.4A CN201811534882A CN109437189A CN 109437189 A CN109437189 A CN 109437189A CN 201811534882 A CN201811534882 A CN 201811534882A CN 109437189 A CN109437189 A CN 109437189A
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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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- 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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
Abstract
The present invention provides a kind of preparation of resin based sphere active carbon and application method, more particularly to chemical technology field, using macropore strong acid cation exchanger resin D001 as active carbon precursor, by being carbonized in a nitrogen atmosphere after the pretreatment such as sieving, washing, then sample is activated using chemical activating agent KOH, finally obtain the small resin based sphere active carbon of a series of smooth surfaces, regular shape, high mechanical strength, fluid resistance, the preparation method is simple, production cost is low, provides fundamental basis for the recycling of waste resin.Active carbon produced by the present invention shows preferably to adsorb desulfurization effect to the simulation fuel oil that dibenzothiophenes (DBT) is target contaminant, 1kg RCS-1 can handle 72L and simulate fuel oil to sulphur concentration 1mg/L or less, it can effectively realize that deep desulfuration, absorption property are greatly improved compared with business active carbon from coal F400.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to a kind of preparation of resin based sphere active carbon and application method.
Background technique
Active carbon not only has biggish specific surface area and flourishing pore structure, also has unique surface chemistries
Matter.Active carbon is divided into Powdered Activated Carbon, granular activated carbon, active carbon fibre peacekeeping spherical activated charcoal by shape difference.Spheric active
Charcoal is the novel absorption material to grow up after powder, particle and fibrous activated carbon, and mainly there are asphaltic base, coal in source
Base and macromolecule resin based raw material, have the characteristics that smooth surface, regular shape, high mechanical strength.Uniform spherical structure makes
Its packed density in fixed bed applications is uniform, and fluid resistance is small, and degree of scatter is preferable in water treatment procedure.Therefore, spherical
The exploitation of absorbent charcoal material has become one of the hot spot direction of Carbon Materials research.Patent No. CN98115717.3 discloses one kind
The preparation method of phenolic resin base globe activated char is raw material using linear thermoplastic's phenolic resin, by adding before balling-up
Enter curing agent, eliminates the non-fusible process of oxidation that asphalt-base spherical activated carbon is prepared as raw material using pitch, obtain partial size and exist
2mm or so and the phenolic resin base globe activated char being evenly distributed.Patent No. CN103936004B is by phenols and aldehydes according to one
Fixed molar ratio mixing, is added phenol catalysis agent and dispersing agent, and phenols curing agent and pore creating material, filtering is added after continuing stirring
Resin balls are obtained, then are carbonized under nitrogen protection, then activated, room temperature is cooled to, obtain the spherical activity of phenolic resin base
Charcoal.Patent No. CN100417590C is steamed so that spherical resin is commercialized as raw material by air oxidation, then through high temperature cabonization and water
Gas activation prepares spherical activated charcoal.
In recent years, in fuel desulfuration technical field, the technologies such as traditional hydrodesulfurization, biological desulphurization, oxidation sweetening exist
Certain limitation, absorption desulfurization technology is since operating condition is mild, expense is low, does not reduce olefin(e) centent and octane in oil product
The features such as deep desulfuration can be achieved in value, is widely studied.Active carbon passes through physical absorption and thiophene-based as adsorbent
Testing sulphide interaction, absorption property are mainly to be determined by its surface texture properties and surface chemical property.Active carbon is rich
Rich pore structure and bigger serface makes its absorption property be better than molecular sieve, metal oxide etc., wherein micropore and central hole structure
Its adsorbance and adsorption dynamics adsorption kinetics to thiophene-type sulfide is even more affected respectively.
Existing active charcoal preparing process step is complicated, and activated carbon pore size distribution is uncontrollable；Active carbon specific surface area and hole
Hold relatively low；And the disadvantages of adsorbent sweetening process operating condition is harsh, and operating cost is high, and adsorption capacity is relatively limited.
In view of the above deficiencies, now need a kind of method for preparing resin based sphere active carbon with more sufficient the deficiencies in the prior art.
Summary of the invention
It is an object of the invention to provide a kind of preparation of resin based sphere active carbon and application methods, and not only preparation method is simple,
Production cost is low, provides fundamental basis for the recycling of waste resin；And active carbon regular shape, high mechanical strength can lead to
It crosses preparation condition effectively to regulate and control active carbon internal structure, active carbon shows higher suction to DBT in simulation fuel oil
Attached capacity and preferable adsorptive selectivity, absorption desulfurization performance are far superior to commercial activated carbons.
The present invention provides the following technical solutions:
A kind of method for preparing resin based sphere active carbon, steps are as follows:
The pretreatment of S1, precursor macropore strong acid cation exchanger resin D001: D001 is sieved to 0.50- using preceding
Then the particle size of 0.63 mm is successively washed with 5%NaOH, deionized water, 5%HCl, deionized water to remove in resin
Residue, clean for several times to neutral, then infiltrated with ethyl alcohol, 60 DEG C are dried for standby repeatedly；
S2, carbonization: the carbonization of active carbon and activation process carry out in high temperature process furnances.Weigh a certain number of D001
It is placed in tube furnace, in N2It is carbonized under atmosphere, N2Flow is 150cm3/min, is risen to the heating rate of 5 DEG C/min by room temperature
Certain carburizing temperature, constant temperature for a period of time, take out when in-furnace temperature is lower than 200 DEG C, obtain a series of samples；
S3, activation: sample is activated using chemical activation method.Using KOH as activator, by sample and KOH in nickel boat
In mixed by certain mass ratio, 5g distilled water, which is added, both to be made to be sufficiently mixed, with identical N2 flow and heating rate by
Room temperature rises to different activation temperatures, activates different time, finally obtains a series of resin based sphere active carbons.
Preferably, in S2 step, carburizing temperature is 500-700 DEG C, carbonization time 0.5-1.5h, and activation time is
0.25-1.5 h。
A kind of resin based sphere active carbon application method is as follows: using containing dibenzothiophenes (DBT) normal octane solution as
Simulation oil, adsorption temp is 25-60 DEG C, adsorption time 2-24h, oil ratio 2.5-10g/L.
To the characterization of resin matrix activated carbon absorption desulfurization effect of the invention, specific assay method is as follows:
S1a, the active carbon for weighing certain mass are added separately to the mould that 25mL initial concentration is 500-2000mg/L DBT
In quasi- oil, after 25 DEG C of constant temperature oscillations reach balance, the DBT concentration of solution after measurement absorption.With DBT in solution when adsorption equilibrium
Concentration CeFor abscissa, adsorbent adsorbance q when adsorption equilibriumeAdsorption isotherm is drawn for ordinate；
S2a, the active carbon for weighing certain mass are placed in the model gasoline that 50mL concentration is 50mg/L DBT, at 25 DEG C
Constant temperature oscillation measures the DBT concentration in solution at regular intervals, until concentration is no longer changed and reaches balance.With absorption
Time t is abscissa, and adsorbance qt is that ordinate draws curve of adsorption kinetics；
S3a, the active carbon for weighing certain mass are fitted into the adsorption column of Φ 1cm × 12cm, and concentration is then added and is
The DBT solution of 1000mg/L, the flow velocity at 25 DEG C with 4BV/h pass through adsorbent, and every 2BV picks up a sample, survey
The concentration of fixed each sample, calculates adsorption capacity.With bed volume (BV) for abscissa, Ce/C0Adsorption penetration is drawn for ordinate
Curve.
Beneficial effects of the present invention:
Method for preparing resin based sphere active carbon of the invention is simple, and production cost is low, mentions for the recycling of waste resin
For theoretical basis；Active carbon regular shape of the invention, high mechanical strength can be by preparation condition to active carbon internal structure
Effectively regulated and controled；Active carbon of the invention shows higher adsorption capacity and preferable absorption to DBT in simulation fuel oil
Selectivity, absorption desulfurization performance are far superior to commercial activated carbons.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the adsorption isotherm of active carbon prepared by embodiment 1-5 and F400 to DBT；
Fig. 2 is the curve of adsorption kinetics of active carbon prepared by embodiment 1-5 and F400 to DBT；
Fig. 3 is the adsorption breakthrough curve of active carbon prepared by embodiment 2 and F400 to DBT；
Fig. 4 resin based sphere active carbon SEM phenogram；
Fig. 5 resin based sphere active carbon SEM characterizes Local map.
Specific embodiment
Embodiment 1
The D001 for weighing certain mass is placed in tube furnace, in N2It is carbonized under atmosphere, N2Flow is 150cm3/min, with 5
DEG C/heating rate of min rises to 600 DEG C of carburizing temperature by room temperature, constant temperature 1h takes out when in-furnace temperature is lower than 200 DEG C,
Then using KOH as activator, mixed in nickel boat in the activation ratio of 0.5 (mass ratio of activator KOH and carbonized samples)
It closes, 5g distilled water, which is added, both to be made to be sufficiently mixed, and 800 DEG C of activation is risen to by room temperature with identical N2 flow and heating rate
Temperature activates 0.5h, obtains resin based sphere active carbon, be denoted as RCS-0.5.
Embodiment 2
With embodiment 1, difference from Example 1 is that activation ratio is 1, obtains resin based sphere active carbon, is denoted as
RCS-1。
Embodiment 3
With embodiment 1, difference from Example 1 is that activation ratio is 2, obtains resin based sphere active carbon, is denoted as
RCS-2。
Embodiment 4
With embodiment 1, difference from Example 1 is that activation ratio is 3, obtains resin based sphere active carbon, is denoted as
RCS-3。
Embodiment 5
With embodiment 1, difference from Example 1 is that activation ratio is 3, obtains resin based sphere active carbon, is denoted as
RCS-4.The specific surface area and pore structure of active carbon prepared by embodiment 1-5 are as shown in table 1, wherein Vt, Vexra-micro,
Vmicro, Vmeso respectively indicate the total pore volume of active carbon, ultramicropore (r < 0.8nm) Kong Rong, micropore (0.8 nm < r < 2nm) Kong Rong
And mesoporous (2nm < r < 50nm) Kong Rong.As shown in Table 1, the hole knot abundant based on microcellular structure is formd inside active carbon
Structure, specific surface area and total pore volume reach as high as 2696m2/g and 1.460cm3/g, when the ratio of activation is smaller, sample aperture master
It embodies a concentrated reflection of as the ultra micro hole number centered on 0.6nm, with the increase of activation ratio, pore size distribution range gradually broadens,
Ultramicropore hole holds the hole number for being gradually reduced and being greater than 2nm and increases.In addition, F400 is a kind of common business active carbon from coal,
Its structural property parameter is equally shown in Table 1.
Embodiment 6
The activated carbon sample and F400 sample for weighing 0.1g embodiment 1-5 preparation are added separately to 20mL initial concentration and are
In the simulation oil of 500,800,1200,1500,2000mg/L DBT, in closed container 25 DEG C of constant temperature oscillations for 24 hours after, measurement
The DBT concentration of solution, the adsorption isotherm of drafting are shown in Fig. 1 after absorption.As shown, active carbon of the invention is to simulation fuel oil
In DBT show higher adsorption capacity, up to about 230mg/g, significantly larger than commercial activated carbons F400.And phase
Than in specific surface area, ultramicropore holds between sample adsorption capacity there are good linear relationship, and micropore filling acts on activity
Important function is played during charcoal absorption DBT.
Embodiment 7
It is 50 mg/L that the activated carbon sample and F400 sample for weighing 0.05g embodiment 1-5 preparation, which are respectively placed in 50mL concentration,
In the model gasoline of DBT, constant temperature oscillation at 25 DEG C measures the DBT concentration in solution at regular intervals, until concentration is no longer
It changes and reaches balance, the curve of adsorption kinetics of drafting is shown in Fig. 2.Active carbon prepared by the present invention shows to inhale faster
Attached diffusion rate, and the rate of adsorption of RCS-3 and RCS-4 with larger mesopore volume is all larger than other samples, shows
Hole controls the adsorption dynamics adsorption kinetics of DBT to a certain extent.
Embodiment 8
The activated carbon sample and F400 sample for weighing the preparation of 5mL embodiment 2 are fitted into the adsorption column of Φ 1cm × 12cm, so
The DBT solution that concentration is 1000mg/L is added afterwards, the flow velocity at 25 DEG C with 4BV/h passes through adsorbent, every 2BV
A sample is picked up, the concentration of each sample is measured, the adsorption breakthrough curve of drafting is shown in Fig. 3.As seen from the figure, compare F400 and
Speech, the working sulfur capacity of RCS-1 are 72.3mg/g, and saturation Sulfur capacity is 17.2mg/g, can produce about 72cm3/g hexichol after column
Bithiophene concentration be lower than 1mg/L low-sulfur solution, i.e. 1kg RCS-1 can handle 72L simulation fuel oil to sulphur concentration 1mg/L hereinafter,
It can effectively realize deep desulfuration；
The specific surface area and pore volume of 1 active carbon of table
These are only the preferred embodiment of the present invention, is not intended to restrict the invention, although with reference to the foregoing embodiments
Invention is explained in detail, for those skilled in the art, still can be to foregoing embodiments institute
The technical solution of record is modified or equivalent replacement of some of the technical features.It is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of resin based sphere active carbon, which is characterized in that steps are as follows:
The pretreatment of S1, precursor macropore strong acid cation exchanger resin D001: D001 is sieved to 0.50-0.63mm using preceding
Particle size, then successively washed with 5%NaOH, deionized water, 5%HCl, deionized water to remove the residual in resin
Object is cleaned for several times to neutrality repeatedly, is then infiltrated with ethyl alcohol, 60 DEG C are dried for standby；
S2, carbonization: the carbonization of active carbon and activation process carry out in high temperature process furnances, weigh a certain number of D001 and are placed in
It in tube furnace, is carbonized under N2 atmosphere, N2 flow is 150cm3/min, is risen to centainly with the heating rate of 5 DEG C/min by room temperature
Carburizing temperature, constant temperature for a period of time, when in-furnace temperature be lower than 200 DEG C when take out, obtain a series of samples；
S3, activation: sample is activated using chemical activation method.Using KOH as activator, sample and KOH are pressed in nickel boat
Certain mass ratio is mixed, and 5g distilled water, which is added, is sufficiently mixed the two, with identical N2 flow and heating rate by room temperature
Different activation temperatures is risen to, different time is activated, finally obtains a series of resin based sphere active carbons.
2. a kind of preparation method of resin based sphere active carbon according to claim 1, which is characterized in that in S2 step,
Carburizing temperature is 500-700 DEG C；Carbonization time is 0.5-1.5h.
3. a kind of preparation method of resin based sphere active carbon according to claim 1, which is characterized in that in S3 step,
The mass ratio of sample and activator KOH are 1:0.5-1:4；Activation time is 0.25-1.5h.
4. a kind of application method of resin based sphere active carbon, which is characterized in that molten with the normal octane containing dibenzothiophenes (DBT)
Liquid investigates absorption of the active carbon to DBT as simulation oil under certain adsorption temp, adsorption time and certain oil ratio example
Performance；Wherein, adsorption temp is 25-60 DEG C；Adsorption time is 2-24h；Oil ratio is 2.5-10g/L.
5. a kind of application method of resin based sphere active carbon according to claim 4, which is characterized in that pass through absorption etc.
Warm line, curve of adsorption kinetics and adsorption breakthrough curve characterize active carbon to the adsorption effect of DBT.
6. a kind of application method of resin based sphere active carbon according to claim 5, which is characterized in that adsorption isotherm
Drawn by the following method: it is 500- that the adsorbent for accurately weighing certain mass, which is added separately to 25mL initial concentration,
In the simulation oil of 2000mg/L DBT, after 25 DEG C of constant temperature oscillations reach balance in closed container, the DBT of solution after measurement absorption
Concentration.Using DBT concentration C e in solution when adsorption equilibrium as abscissa, adsorbent adsorbance qe is that ordinate is made when adsorption equilibrium
Figure, can be obtained active carbon to the adsorption isotherm of DBT.
7. the characterization of adsorption effect of activated carbon in water according to claim 5, it is characterised in that curve of adsorption kinetics is by following
Method is drawn: the sample of sorbent for accurately weighing certain mass is placed in the model gasoline that 50mL concentration is 50mg/L DBT
In, constant temperature oscillation at 25 DEG C measures the DBT concentration in solution at regular intervals, until concentration is no longer changed and reaches flat
Weighing apparatus.Using adsorption time t as abscissa, adsorbance qt is ordinate mapping, and curve of adsorption kinetics can be obtained.
8. the characterization of adsorption effect of activated carbon in water according to claim 5, it is characterised in that adsorption breakthrough curve is pressed with lower section
Method is drawn: the adsorbent for accurately weighing certain mass is fitted into the adsorption column of Φ 1cm × 12cm, and concentration is then added and is
The DBT solution of 1000mg/L, the flow velocity at 25 DEG C with 4BV/h pass through adsorbent, and every 2BV picks up a sample, when
Exit concentration is out of service when being more than initial concentration, measures the concentration of each sample, calculates adsorption capacity.It is with bed volume (BV)
Abscissa, Ce/C0 are ordinate mapping, obtain adsorption breakthrough curve.
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| CN110975325A (en) * | 2019-10-23 | 2020-04-10 | 武汉科技大学 | Method for evaluating adsorption stability of heavy metal ion adsorbent based on solid-phase extraction |
| CN112915966A (en) * | 2021-01-28 | 2021-06-08 | 东北大学 | Preparation method and application of polyaniline-based activated carbon |
| CN113842948A (en) * | 2021-09-24 | 2021-12-28 | 贵州大学 | Nano phenolic resin-based desulfurization catalyst and preparation method thereof |
| CN114713193A (en) * | 2022-04-21 | 2022-07-08 | 华南师范大学 | Nitrogen-doped magnetic porous carbon composite material and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110975325A (en) * | 2019-10-23 | 2020-04-10 | 武汉科技大学 | Method for evaluating adsorption stability of heavy metal ion adsorbent based on solid-phase extraction |
| CN112915966A (en) * | 2021-01-28 | 2021-06-08 | 东北大学 | Preparation method and application of polyaniline-based activated carbon |
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| CN114713193A (en) * | 2022-04-21 | 2022-07-08 | 华南师范大学 | Nitrogen-doped magnetic porous carbon composite material and preparation method and application thereof |
| CN114713193B (en) * | 2022-04-21 | 2023-11-14 | 华南师范大学 | Nitrogen-doped magnetic porous carbon composite material and preparation method and application thereof |
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