CN105110330B - Preparation method for activated carbon material and application thereof - Google Patents
Preparation method for activated carbon material and application thereof Download PDFInfo
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Abstract
The invention provides a preparation method for an activated carbon material. The preparation method comprises the following steps: 1) taking an activator aqueous solution, adding ion exchange resin and stirring and mixing the mixture for ion exchange; 2) washing, filtering and drying the obtained mixture to obtain the required resin; 3) optional one step: a, carbonizing the obtained resin in an N2 atmosphere; b, after pre-oxidizing the obtained resin in air, carbonizing the resin in the N2 atmosphere; and 4) washing and drying the obtained carbon material to obtain the required activated carbon material. The invention further discloses an activated carbon material by adopting the method and application thereof. According to the activated carbon material and the application thereof provided by the invention, the activator can be uniformly dispersed and the carbon material is activated by alkali metal ions at a high temperature. The prepared activated carbon material has good application potential in adsorbing carbon dioxide and phenol.
Description
Technical field
The invention belongs to chemical field, it is related to a kind of preparation method and applications of absorbent charcoal material, and in particular to a kind of
The preparation method of high performance active carbon material is prepared and its in carbon dioxide, Adsorption of Phenol side as presoma with ion exchange resin
The application in face.
Background technology
Activated carbon has the advantages that cheap, chemical stability is good, specific surface area is big, absorption, separate, the neck such as catalysis
Domain is had a wide range of applications, and it is prepared mainly by charcoal, wood chip, coconut husk, fruit stone, polymer, coal and heavy crude etc.
It is obtained through carbonization-activation, wherein activation process has important influence for the pore passage structure of activated carbon, and finally determines
Performance of the material in intended application field is good and bad.
The activation method of current carbon material mainly includes physical activation method, chemical activation method and multiplicity reactivation method：(1) physics
Activation method mainly has steam activation method and carbon dioxide activation method, such as B.G.Prakash Kumar et al. (Journal of
Hazardous Materials,2006.B136:P.922-929) with sawdust as raw material, water vapour be activator in 600-
The absorbent charcoal material with large specific surface area has been prepared at 750 DEG C；(2) chemical activation method mainly has base reagent activation method
(as using KOH activation), (such as patent CN201210171210.8 is by longan shell in 30-60wt% for acids reagent activation method
H3PO4Impregnated in solution, prepared after 550-650 DEG C of carbonization-activation specific surface area it is big, to methylene blue/iodine advantages of good adsorption effect
Absorbent charcoal material) and salt reagent activation method (such as patent CN201110351784.9 by stalk 20-50wt% ZnCl2It is molten
Impregnated 20-30 hours in liquid, high temperature cabonization activation finally gives absorbent charcoal material)；(3) multiplicity reactivation method, will be physically activated
The activation method being combined with chemical activation.
Wherein, compared to physical activation method and multiplicity reactivation method, the related process of chemical activation method is more ripe, especially with
KOH is most widely used for activator.At present, the feed postition of KOH mainly has two kinds in activation process：(1) by letter
Single solid mixing, the solid material powder of physical mixed and KOH powder is activated at high temperature, such as Muniandy
(Microporous and Mesoporous Materials,2014.197:) and (ACS such as Chen, Z.H p.316-323
Applied Materials&Interfaces,2013.5(15):P.6937-6945.) it is the warp with KOH powder as activator
The absorbent charcoal material that specific surface area is big, micro content is high, carbon dioxide adsorption performance is good is prepared after different temperatures carbonization-activation；
(2) KOH is configured to certain density solution in advance, by the method that impregnates by KOH physical depositions in carbon material (or carbon material
Presoma) duct in, such as I.A.W.Tan et al. (Chemical Engineering Journal, 2007.127:p.111–
119) after the carbon material obtained by oil palm fibre carbonization being impregnated into a certain amount of KOH, high-temperature activation has prepared energy at 850 DEG C
The activated carbon of a large amount of absorption methylene blues.However, either preparing the mistake of activated carbon using the method for solid mixing or dipping
All there is activator situation pockety in journey, this means that activation process is difficult in carbon skeleton uniformly carry out.
Therefore, the deficiency for existing for above-mentioned activated carbon chemical activating process, it is necessary to explore new raw material new
Preparation method and its under the conditions of prepare absorbent charcoal material, so as to be effectively improved the activation effect of activated carbon.
The content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of preparation side of absorbent charcoal material
Method and its application, for solving the problems, such as that absorbent charcoal material is in chemical activating process in the prior art, so as to improve activity
Application of the Carbon Materials in fields such as carbon dioxide adsorption, Adsorption of Phenol.
In order to achieve the above objects and other related objects, first aspect present invention provides a kind of preparation of absorbent charcoal material
Method, specifically includes following steps：
1) the activator aqueous solution is taken, ion exchange resin is added, ion exchange is carried out after stirring mixing；
Preferably, the activator is selected from Ca (NO3)2、CaCl2、Mg(NO3)2、MgCl2、NaOH、NaCl、NaNO3、KOH、
KCl、KNO3In any one.It is highly preferred that the activator is KOH.
Preferably, the concentration of the activator aqueous solution is 0.1-5mol/L.
Preferably, the ion exchange resin be selected from D001 (large hole strong acid styrene system cation exchange resin),
D113 (macropore acidulous acrylic acid's cation exchanger resin), 001 × 7 (degree of cross linking is 7 strongly acidic styrene's cation
Exchanger resin), 732 (strongly acidic styrene type cation exchange resins), D751 (chelating type cationic ion-exchange resin) ion hand over
Change any one in resin.It is highly preferred that the ion exchange resin is that 001 × 7 (degree of cross linking is 7 strongly acidic styrene
Cation exchanger resin) ion exchange resin.
The ion exchange resin is activated carbon precursor.The D001, D113,001 × 7,732, D751 ion exchanges
Resin is commercialized ion exchange resin that can be commercially available.Wherein, D001 refers to macropore strong acid polystyrene sun
Ion exchange resin, D113 refers to macropore acidulous acrylic acid's cation exchanger resin, and 001 × 7 finger degree of cross linking is 7 highly acid
Styrene type cation exchange resin, 732 refer to strongly acidic styrene type cation exchange resin, and D751 refers to that chelating type cation is handed over
Change resin.
Preferably, the ion exchange resin and the volume ratio of the activator aqueous solution are 1：0.1-2.It is highly preferred that described
Ion exchange resin is 1 with the volume ratio of the activator aqueous solution：2.
Preferably, the stirring condition is：Whipping temp：20-40℃；Mixing time：6-72 hours；Change activator water
The time of solution：2-24 hours.Need to change an activator aqueous solution at interval of a period of time during the stirring.
It is highly preferred that the stirring condition is：Whipping temp：30℃；Mixing time：32 hours；Change activator water-soluble
The time of liquid：8 hours.
2) by step 1) obtained by mixture washed, filter after dry, obtain final product required resin；
Preferably, the washing is washed to neutrality mixture using deionized water.The pH of the mixture is 6.8-
7.2。
It is described to be filtered into conventional filtration mode.The filtering is will to wash to have neither part nor lot in ion exchange to neutral mixture
Ion filter removal.
Preferably, the drying temperature is 80-150 DEG C.It is highly preferred that the drying temperature is 100 DEG C.
Preferably, the resin is the resin of dopant activation agent neutral and alkali metal ion.
3) selected from following any：
A. by step 2) resulting resin is processed in N2It is carbonized under atmosphere；
Preferably, the Carbonization Conditions are：N2Flow：30-200mL/min；Carburizing temperature：300-1000℃；Heat up speed
Rate：1-10℃/min；Carbonization time：0.5-6 hours.
It is highly preferred that the Carbonization Conditions are：N2Flow：100mL/min；Carburizing temperature：500-800℃；Heating rate：
5℃/min；Carbonization time：3 hours.
B. by step 2) after the resin obtained by treatment pre-oxidizes in atmosphere, then in N2It is carbonized under atmosphere；
Preferably, the pre-oxidizing conditions are：Air mass flow：30-200mL/min；Pre oxidation：100-300℃；Rise
Warm speed：1-10℃/min；Preoxidation time：0.5-6 hours.
It is highly preferred that the pre-oxidizing conditions are：Air mass flow：100mL/min；Pre oxidation：200℃；Heat up speed
Rate：5℃/min；Preoxidation time：1 hour.
Preferably, the Carbonization Conditions are：N2Flow：30-200mL/min；Carburizing temperature：300-1000℃；Heat up speed
Rate：1-10℃/min；Carbonization time：0.5-6 hours.
It is highly preferred that the Carbonization Conditions are：N2Flow：100mL/min；Carburizing temperature：500-800℃；Heating rate：
5℃/min；Carbonization time：3 hours.
Preferably, in step a, b, the consumption of the resin is 3-15g.It is highly preferred that the consumption of the resin is
10g。
For different resins, can select to be carbonized using a kind of mode in step a, b, wherein, some resins are adopted
With first pre-oxidizing before carbonization, effect is more preferable.
4) by step 3) obtained by carbon material washing after dry, obtain final product required absorbent charcoal material.
Preferably, after the washing is first washed using aqueous hydrochloric acid solution, then carbon material is washed into using deionized water
Property.
It is highly preferred that the concentration of the aqueous hydrochloric acid solution is 0.05-2mol/L.Most preferably, the aqueous hydrochloric acid solution
Concentration is 0.1mol/L.
It is highly preferred that the wash time of the aqueous hydrochloric acid solution is 1-6 hours.Most preferably, the aqueous hydrochloric acid solution
Wash time is 2 hours.
Preferably, the drying temperature is 80-150 DEG C.It is highly preferred that the drying temperature is 100 DEG C.
The absorbent charcoal material can keep the spherical design of original ion exchange resin, also ground can obtain powdered work
Property Carbon Materials.
Second aspect present invention is also disclosed using a kind of prepared absorbent charcoal material for obtaining of the above method.
Third aspect present invention further discloses a kind of absorbent charcoal material obtained using the above method to two
Application on carbonoxide, Adsorption of Phenol.
As described above, the invention discloses a kind of preparation method of absorbent charcoal material, being with cheap ion exchange resin
Presoma, alkaline metal ionses are activator, successively obtain duct highly by pretreatment, Low Temperature Heat Treatment, high-temperature heat treatment
Flourishing absorbent charcoal material.In the present invention, activator can realize quasi- ion level in carbon materials material precursor (or carbon material)
High uniformity disperses, and uniform activation effect of the alkaline metal ionses to carbon material under high temperature is realized, so as to be effectively improved activation effect
Really.Preparation method low cost involved in the present invention, synthesis technique is simple, it is easy to amplify.
Prepared absorbent charcoal material specific surface area of the invention is big, and micro content is high, and ion exchange resin can be kept original
Sphericity, associated materials have the key characters such as adsorption capacity is big, the rate of adsorption is fast during carbon dioxide and Adsorption of Phenol,
There is preferable absorption property to carbon dioxide and phenol, have broad application prospects.
Specific embodiment
The present invention is expanded on further with reference to specific embodiment, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention.
Embodiments of the present invention are illustrated below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages of the invention and effect easily.The present invention can also be by specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
It should be clear that the reagent used in following examples for example activator, ion exchange resin, wash solution can be from the market
Purchase.Not specific dated process equipment or device use conventional equipment or device in the art in the following example；Institute
There are pressure value and scope all referring to relative pressure.
In addition, it is to be understood that one or more method and steps mentioned in the present invention do not repel before and after the combination step
Can also there is other method step or other method step can also be inserted between the step of these are specifically mentioned, unless separately
It is described；It should also be understood that the combination annexation between one or more the equipment/devices mentioned in the present invention is not repelled
Can also exist before and after the unit equipment/device other equipment/device or two equipment/devices specifically mentioning at these it
Between can also insert other equipment/device, unless otherwise indicated.And, unless otherwise indicated, the numbering of various method steps is only
Differentiate the convenient tool of various method steps, rather than to limit the ordering of various method steps or limiting enforceable model of the invention
Enclose, being altered or modified for its relativeness is of the invention enforceable when being also considered as in the case of without essence change technology contents
Category.
Embodiment 1
It is by volume 1:It is the KOH aqueous solution of 1mol/L that 2 ratio measures 001 × 7 ion exchange resin and concentration,
30 DEG C of stirrings mix 32 hours, and change a KOH solution at interval of 8 hours.And after washed to neutrality through deionized water, filtering
Afterwards, it is dried to obtain K at 100 DEG C+Doping resin.Take 10gK+Doping resin is the N of 100mL/min in flow2Lower 500 DEG C of atmosphere
Carbonization 3 hours, heating rate is 5 DEG C/min.Then, the carbon material of above-mentioned preparation is first washed from the HCl solution of 0.1mol/L
Wash 2 hours, then washed to neutrality through deionized water, dry prepared absorbent charcoal material sample 1# after filtering at 100 DEG C.Activated carbon
The texture property of material sample 1# is shown in Table 1.
Embodiment 2
It is by volume 1:It is the KOH aqueous solution of 1mol/L that 2 ratio measures 001 × 7 ion exchange resin and concentration,
30 DEG C of stirrings mix 32 hours, and change a KOH solution at interval of 8 hours.And after washed to neutrality through deionized water, filtering
Afterwards, it is dried to obtain K at 100 DEG C+Doping resin.Take 10gK+Doping resin is first in flow for 200 DEG C in the air of 100mL/min
After pre-oxidation 1 hour, then it is the N of 100mL/min in flow2Lower 500 DEG C of atmosphere is carbonized 3 hours, and heating rate is 5 DEG C/min.
Then, the carbon material of above-mentioned preparation is first washed 2 hours from the HCl solution of 0.1mol/L, then is washed into through deionized water
Property, prepared absorbent charcoal material sample 2# is dried after filtering at 100 DEG C.The texture property of absorbent charcoal material sample 2# is shown in Table 1.
Embodiment 3
It is by volume 1:It is the KOH aqueous solution of 1mol/L that 2 ratio measures 001 × 7 ion exchange resin and concentration,
30 DEG C of stirrings mix 32 hours, and change a KOH solution at interval of 8 hours.And after washed to neutrality through deionized water, filtering
Afterwards, it is dried to obtain K at 100 DEG C+Doping resin.Take 10gK+Doping resin is the N of 100mL/min in flow2Lower 600 DEG C of atmosphere
Carbonization 3 hours, heating rate is 5 DEG C/min.Then, the carbon material of above-mentioned preparation is first washed from the HCl solution of 0.1mol/L
Wash 2 hours, then washed to neutrality through deionized water, dry prepared absorbent charcoal material sample 3# after filtering at 100 DEG C.Activated carbon
The texture property of material sample 3# is shown in Table 1.
Embodiment 4
It is by volume 1:It is the KOH aqueous solution of 1mol/L that 2 ratio measures 001 × 7 ion exchange resin and concentration,
30 DEG C of stirrings mix 32 hours, and change a KOH solution at interval of 8 hours.And after washed to neutrality through deionized water, filtering
Afterwards, it is dried to obtain K at 100 DEG C+Doping resin.Take 10gK+Doping resin is first in flow for 200 DEG C in the air of 100mL/min
After pre-oxidation 1 hour, then it is the N of 100mL/min in flow2Lower 600 DEG C of atmosphere is carbonized 3 hours, and heating rate is 5 DEG C/min.
Then, the carbon material of above-mentioned preparation is first washed 2 hours from the HCl solution of 0.1mol/L, then is washed into through deionized water
Property, prepared absorbent charcoal material sample 4# is dried after filtering at 100 DEG C.The texture property of absorbent charcoal material sample 4# is shown in Table 1.
Embodiment 5
It is by volume 1:It is the KOH aqueous solution of 1mol/L that 2 ratio measures 001 × 7 ion exchange resin and concentration,
30 DEG C of stirrings mix 32 hours, and change a KOH solution at interval of 8 hours.And after washed to neutrality through deionized water, filtering
Afterwards, it is dried to obtain K at 100 DEG C+Doping resin.Take 10gK+Doping resin is the N of 100mL/min in flow2Lower 700 DEG C of atmosphere
Carbonization 3 hours, heating rate is 5 DEG C/min.Then, the carbon material of above-mentioned preparation is first washed from the HCl solution of 0.1mol/L
Wash 2 hours, then washed to neutrality through deionized water, dry prepared absorbent charcoal material sample 5# after filtering at 100 DEG C.Activated carbon
The texture property of material sample 5# is shown in Table 1.
Embodiment 6
It is by volume 1:It is the KOH aqueous solution of 1mol/L that 2 ratio measures 001 × 7 ion exchange resin and concentration,
30 DEG C of stirrings mix 32 hours, and change a KOH solution at interval of 8 hours.And after washed to neutrality through deionized water, filtering
Afterwards, it is dried to obtain K at 100 DEG C+Doping resin.Take 10gK+Doping resin is first in flow for 200 DEG C in the air of 100mL/min
After pre-oxidation 1 hour, then it is the N of 100mL/min in flow2Lower 700 DEG C of atmosphere is carbonized 3 hours, and heating rate is 5 DEG C/min.
Then, the carbon material of above-mentioned preparation is first washed 2 hours from the HCl solution of 0.1mol/L, then is washed into through deionized water
Property, prepared absorbent charcoal material sample 6# is dried after filtering at 100 DEG C.The texture property of absorbent charcoal material sample 6# is shown in Table 1.
Embodiment 7
It is by volume 1:It is the KOH aqueous solution of 1mol/L that 2 ratio measures 001 × 7 ion exchange resin and concentration,
30 DEG C of stirrings mix 32 hours, and change a KOH solution at interval of 8 hours.And after washed to neutrality through deionized water, filtering
Afterwards, it is dried to obtain K at 100 DEG C+Doping resin.Take 10gK+Doping resin is the N of 100mL/min in flow2Lower 800 DEG C of atmosphere
Carbonization 3 hours, heating rate is 5 DEG C/min.Then, the carbon material of above-mentioned preparation is first washed from the HCl solution of 0.1mol/L
Wash 2 hours, then washed to neutrality through deionized water, dry prepared absorbent charcoal material sample 7# after filtering at 100 DEG C.Activated carbon
The texture property of material sample 7# is shown in Table 1.
Embodiment 8
It is by volume 1:It is the KOH aqueous solution of 1mol/L that 2 ratio measures 001 × 7 ion exchange resin and concentration,
30 DEG C of stirrings mix 32 hours, and change a KOH solution at interval of 8 hours.And after washed to neutrality through deionized water, filtering
Afterwards, it is dried to obtain K at 100 DEG C+Doping resin.Take 10gK+Doping resin is first in flow for 200 DEG C in the air of 100mL/min
After pre-oxidation 1 hour, then it is the N of 100mL/min in flow2Lower 800 DEG C of atmosphere is carbonized 3 hours, and heating rate is 5 DEG C/min.
Then, the carbon material of above-mentioned preparation is first washed 2 hours from the HCl solution of 0.1mol/L, then is washed into through deionized water
Property, prepared absorbent charcoal material sample 8# is dried after filtering at 100 DEG C.The texture property of absorbent charcoal material sample 8# is shown in Table 1.
The texture property of absorbent charcoal material in the embodiment 1-8 of table 1
Embodiment 9
According to the absorbent charcoal material sample 1-8# prepared in embodiment 1-8, its texture property is shown in Table 1.Can by table 1
Know, the specific surface area of the absorbent charcoal material in the present invention is big, and micro content is high, can have in the method that the present invention prepares activated carbon
The synthesis of effect ground has the absorbent charcoal material of good adsorption effect to small molecule.
The absorbent charcoal material sample 1-8# that will be prepared in embodiment 1-8 carries out the isothermal adsorption of carbon dioxide respectively,
The CO of sample is measured using full-automatic specific surface area and pore analysis instrument2Absorption property, carbon dioxide body gas purity >=
99.99%, adsorption temp is 25 DEG C, and adsorptive pressure is 1bar, absorption duration 3 hours, the isothermal adsorption knot of specific carbon dioxide
Fruit is shown in Table 2.As shown in Table 2, prepared absorbent charcoal material sample 1-8# has shown good CO2Absorption property, particularly its
Middle sample 5-6# is to CO2Adsorbance be better than other samples.
Meanwhile, the phenol that the absorbent charcoal material sample 1-8# of 0.1g is used to adsorb in 200mg/L phenol solutions is taken respectively,
The Adsorption of Phenol performance of sample is measured using full-automatic specific surface area and pore analysis instrument, phenol solution volume is 200mL, absorption
Temperature is 28 DEG C, absorption duration 4 hours, and the isothermal adsorption of absorbent charcoal material sample 1-8# Pyrogentisinic Acids the results are shown in Table 2.Can by table 2
Know, prepared activated carbon sample 1-8# Pyrogentisinic Acids have good adsorption effect, particularly the wherein suction of sample 5-6# Pyrogentisinic Acids
Attached amount is better than other samples.
The carbon dioxide and Adsorption of Phenol performance of the embodiment activated carbon of table 2
Meanwhile, current Commercial active Carbon Materials are under 25 DEG C, 1bar pressure to CO2Adsorbance in 8.0wt% or so, and
From Table 2, it can be seen that absorbent charcoal material is to CO in the present invention2Adsorptivity amount can reach 14.4wt%, be much better than business
The activated carbon of product.Additionally, absorbent charcoal material is also commonly used for the absorption of phenol, absorbent charcoal material of the present invention is in 28 DEG C, 1bar
Under the conditions of the adsorbance of Pyrogentisinic Acid can reach 2.21mmol/g, far above commercialization absorbent charcoal material under equal conditions
The absorption (absorption of commercial activated charcoal Pyrogentisinic Acid under the conditions of 28 DEG C, 1bar is basic in 0.8mmol/g or so) of Pyrogentisinic Acid.Always
It, activated carbon of the present invention not only has originality on its preparation method, while to CO2There is good adsorptivity with phenol
Energy.
Embodiment 10
It is by volume 1:It is the NaOH aqueous solution of 5mol/L that 0.1 ratio measures D001 ion exchange resin and concentration,
Mix 72 hours in 20 DEG C of stirrings, and a NaOH solution was changed at interval of 18 hours.And after washed to neutrality through deionized water,
After filtering, Na is dried to obtain at 80 DEG C+Doping resin.Take 3gNa+Doping resin is the N of 30mL/min in flow2Under atmosphere
300 DEG C are carbonized 6 hours, and heating rate is 1 DEG C/min.Then, by the carbon material of above-mentioned preparation first from the HCl of 0.05mol/L
Solution is washed 6 hours, then is washed to neutrality through deionized water, dries prepared absorbent charcoal material sample after filtering at 80 DEG C.Institute
The absorbent charcoal material sample specific surface area of preparation is big, and micro content is high, with well to carbon dioxide and the adsorption capacity of phenol.
Embodiment 11
It is by volume 1:It is the CaCl of 0.1mol/L that 2 ratio measures D113 ion exchange resin and concentration2The aqueous solution,
Mix 6 hours in 40 DEG C of stirrings, and a CaCl was changed at interval of 1.5 hours2Solution.And after washed into through deionized water
Property, after filtering, Ca is dried to obtain at 150 DEG C2+Doping resin.Take 15g Ca2+Doping resin is the N of 200mL/min in flow2
Lower 1000 DEG C of atmosphere is carbonized 0.5 hour, and heating rate is 10 DEG C/min.Then, the carbon material of above-mentioned preparation is first selected into 2mol/
The HCl solution of L is washed 2 hours, then is washed to neutrality through deionized water, dries prepared absorbent charcoal material after filtering at 150 DEG C
Sample.Prepared absorbent charcoal material sample specific surface area is big, and micro content is high, with suction well to carbon dioxide and phenol
Attached ability.
Embodiment 12
It is by volume 1:It is the Mg (NO of 2mol/L that 1 ratio measures 732 ion exchange resin and concentration3)2The aqueous solution,
Mix 48 hours in 25 DEG C of stirrings, and a Mg (NO was changed at interval of 12 hours3)2Solution.And after washed into through deionized water
Property, after filtering, Mg is dried to obtain at 120 DEG C2+Doping resin.Take 8g Mg2+Doping resin is first 30mL/min's in flow
In air 100 DEG C pre-oxidation 6 hours after, then flow for 150mL/min N2Lower 500 DEG C of atmosphere is carbonized 2 hours, heating rate
It is 3 DEG C/min.Then, the carbon material of above-mentioned preparation is first washed 4 hours from the HCl solution of 0.5mol/L, then through deionization
Water washing dries prepared absorbent charcoal material sample to neutrality at 120 DEG C after filtering.Prepared absorbent charcoal material sample compares table
Area is big, and micro content is high, with well to carbon dioxide and the adsorption capacity of phenol.
Embodiment 13
It is by volume 1:It is the KNO of 1mol/L that 1.5 ratio measures D751 ion exchange resin and concentration3The aqueous solution,
Mix 56 hours in 35 DEG C of stirrings, and a KNO was changed at interval of 14 hours3Solution.And after washed to neutrality through deionized water,
After filtering, K is dried to obtain at 110 DEG C+Doping resin.Take 12gK+Doping resin is first in flow in the air of 200mL/min
After 300 DEG C pre-oxidize 0.5 hour, then it is the N of 120mL/min in flow2Lower 600 DEG C of atmosphere is carbonized 4 hours, and heating rate is 4
℃/min.Then, the carbon material of above-mentioned preparation is first washed 3 hours from the HCl solution of 1.5mol/L, then is washed through deionization
Wash to neutrality, dry prepared absorbent charcoal material sample after filtering at 110 DEG C.Prepared absorbent charcoal material sample specific surface area
Greatly, micro content is high, with well to carbon dioxide and the adsorption capacity of phenol.
So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
The personage for knowing this technology all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should be covered by claim of the invention.
Claims (4)
1. a kind of preparation method of absorbent charcoal material, specifically includes following steps：
1）The activator aqueous solution is taken, ion exchange resin is added, ion exchange is carried out after stirring mixing；
2）By step 1）Resulting mixture washed, filter after dry, obtain final product required resin；
3）Selected from following any：
a）By step 2）Resin obtained by treatment is in N2It is carbonized under atmosphere；
b）By step 2）After resin obtained by treatment is pre-oxidized in atmosphere, then in N2It is carbonized under atmosphere；
4）By step 3）Dried after resulting carbon material washing, obtain final product required absorbent charcoal material；
Step 1）In, the activator is selected from Ca (NO3)2、CaCl2、Mg(NO3)2、MgCl2、NaOH、NaCl、NaNO3、KOH、
KCl、KNO3In any one；
Step 1）In, the ion exchange resin is big selected from D001 large hole strong acid styrene system cation exchange resins, D113
Hole acidulous acrylic acid's cation exchanger resin, the strongly acidic styrene type cation exchange resin that 001 × 7 degree of cross linking is 7,
Any one in 732 strongly acidic styrene type cation exchange resins, D751 chelating type cationic ion-exchange resins；
Step 1）In, the ion exchange resin is 1 with the volume ratio of the activator aqueous solution：0.1-2；
Step 1）In, the stirring condition is：Whipping temp：20-40℃；Mixing time：6-72 hours；Change activator water-soluble
The time of liquid：2-24 hours；
Step a）In, the Carbonization Conditions are：N2Flow：30-200mL/min；Carburizing temperature：300-1000℃；Heating rate：
1-10℃/min；Carbonization time：0.5-6 hours；
Step b）In, the pre-oxidizing conditions are：Air mass flow：30-200mL/min, Pre oxidation：100-300 DEG C, heat up
Speed：1-10 DEG C/min, preoxidation time：0.5-6 hours；The Carbonization Conditions are：N2Flow：30-200mL/min, carbonization
Temperature：300-1000 DEG C, heating rate：1-10 DEG C/min, carbonization time：0.5-6 hours.
2. the preparation method of absorbent charcoal material according to claim 1, it is characterised in that step 4）In, the washing is adopted
After first being washed with aqueous hydrochloric acid solution, then carbon material is washed to neutrality using deionized water.
3. a kind of absorbent charcoal material, is obtained by the preparation method of any described absorbent charcoal materials of claim 1-2.
4. application of the absorbent charcoal material according to claim 3 on to carbon dioxide, Adsorption of Phenol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510504305.0A CN105110330B (en) | 2015-08-17 | 2015-08-17 | Preparation method for activated carbon material and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510504305.0A CN105110330B (en) | 2015-08-17 | 2015-08-17 | Preparation method for activated carbon material and application thereof |
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| CN105664850B (en) * | 2016-01-26 | 2018-06-26 | 中国科学院上海高等研究院 | A kind of preparation method and applications of high performance carbon base carbon dioxide sorbing material |
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| CN106348280A (en) * | 2016-10-21 | 2017-01-25 | 南通绿业中试技术研究院有限公司 | Preparation method for spherical porous carbon |
| CN108079943A (en) * | 2016-11-19 | 2018-05-29 | 曹建涛 | A kind of preparation method with superelevation mesoporous spheric active carbon |
| CN107020070A (en) * | 2017-03-03 | 2017-08-08 | 林志雄 | A kind of gas mask sorbing material |
| CN109019593A (en) * | 2018-09-19 | 2018-12-18 | 东北大学 | A kind of discarded ion exchange resin matrix activated carbon and the preparation method and application thereof |
| CN110182797B (en) * | 2019-03-19 | 2021-02-02 | 杭州电子科技大学 | Preparation method of modified activated carbon material for capacitive deionization technology |
| CN112978707A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | Preparation method of ion exchange resin-based carbon beads |
| CN111249765B (en) * | 2020-02-25 | 2021-04-06 | 中国科学院化学研究所 | Pressurized fluid extraction system and method for removing metal ions from carbon material |
| CN111892069B (en) * | 2020-08-28 | 2022-05-24 | 江苏理工学院 | Needle-shaped C-Na2CO3Preparation method of (1) |
| CN114618432B (en) * | 2020-12-10 | 2023-06-30 | 中国科学院大连化学物理研究所 | Preparation method and application of resin-based carbon microsphere |
| CN114620723A (en) * | 2020-12-10 | 2022-06-14 | 中国科学院大连化学物理研究所 | Preparation method of strong-acid ion exchange resin-based carbon spheres |
| CN112973627B (en) * | 2021-02-08 | 2023-07-28 | 北京工业大学 | Active carbon composite modification method for LAS removal in building grey water |
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| CN113967464B (en) * | 2021-11-04 | 2023-12-01 | 苏州工业园区安泽汶环保技术有限公司 | Preparation method and application of high-purity active carbon material for air purification |
| CN115196726A (en) * | 2022-07-13 | 2022-10-18 | 江苏省环境工程技术有限公司 | Resin-based derivative carbon electrode for electro-adsorption desalination and preparation method thereof |
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